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Небесная энциклопедия

Космические корабли и станции, автоматические КА и методы их проектирования, бортовые комплексы управления, системы и средства жизнеобеспечения, особенности технологии производства ракетно-космических систем

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Мониторинг СМИ

Мониторинг СМИ и социальных сетей. Сканирование интернета, новостных сайтов, специализированных контентных площадок на базе мессенджеров. Гибкие настройки фильтров и первоначальных источников.

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Поддерживает ввод нескольких поисковых фраз (по одной на строку). При поиске обеспечивает поддержку морфологии русского и английского языка
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Применить Всего найдено 13565. Отображено 100.
15-03-2012 дата публикации

Purification of fluoroalkanesulfonate salts

Номер: US20120065425A1
Автор: Allen Capron Sievert, James A. Schultz, Katelyn Rae Walck, Lee Grant Sprague
Принадлежит: EI Du Pont de Nemours and Co

A process for the purification of fluoroalkanesulfonate salt comprising (a) contacting a mixture of said salt and an inorganic salt contaminant with a solvent to selectively dissolve said fluoroalkanesulfonate salt in solution, and (b) isolating the solution, to yield a fluoroalkanesulfonate salt containing less than 500 micrograms of inorganic salt contaminant per gram of fluoroalkanesulfonate salt, or containing less than a maximum of 0.3% by weight of individual solvent.

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Номер записи: 1
29-03-2012 дата публикации

Process for Reducing Inorganics from and Concentrating Anionic Surfactant Solutions

Номер: US20120078008A1
Автор: Edward D. Daugs
Принадлежит: Dow Global Technologies LLC

A process including contacting one or more Strecker sulfonation reaction products of one or more halogenated alkyl ethers in the presence of sulfite with one or more polar water soluble organic solvents selected from acetone, methyl ethyl ketone, the C 2 -C 5 alkyl alcohols, and the like, to form an extraction mixture; allowing the extraction mixture to separate into an aqueous phase and an organic phase; and separating the aqueous phase from the organic phase; wherein the one or more Strecker sulfonation reaction products each comprise at least 30 percent by weight of one or more inorganic salts and the organic phase following separation comprises less than 20 percent by weight of one or more inorganic salts, is provided.

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Номер записи: 2
03-05-2012 дата публикации

Cross-Coupled Peptide Nucleic Acids for Detection of Nucleic Acids of Pathogens

Номер: US20120107794A1
Автор: Christopher Micklitsch, Daniel H. Appella
Принадлежит: US Department of Health and Human Services

The present invention concerns methods for detecting a nucleic acid comprising (i) contacting a solution comprising a first PNA having a first cross-reactive functional group with a substrate having a second PNA affixed thereto, the second PNA having a second first cross-reactive functional group, wherein the first PNA has a reporter molecule attached thereto and the first and second PNAs being complementary to different portions of a target DNA; (ii) contacting a sample suspected of containing the nucleic acid with the first and second PNAs; and (iii) determining the presence of the reporter molecule on the substrate.

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Номер записи: 3
10-05-2012 дата публикации

Fluorosurfactants

Номер: US20120111233A1
Автор: Andreas Bathe, Eckhard Claus, Jan Krause, Melanie Kleineidam, Steffen Schellenberger, Wolfgang Hierse
Принадлежит: Merck Patent GmBH

The present invention relates to novel compounds containing fluorinated end groups, to the use thereof as surface-active substances, and to processes for the preparation of these compounds.

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Номер записи: 4
24-05-2012 дата публикации

Sulfonium salt-containing polymer, resist composition, patterning process, and sulfonium salt monomer and making method

Номер: US20120129103A1
Автор: Jun Hatakeyama, Masaki Ohashi, Seiichiro Tachibana, Youichi Ohsawa
Принадлежит: Shin Etsu Chemical Co Ltd

A sulfonium salt having a 4-fluorophenyl group is introduced as recurring units into a polymer comprising hydroxyphenyl (meth)acrylate units and acid labile group-containing (meth)acrylate units to form a polymer which is useful as a base resin in a resist composition. The resist composition has a high sensitivity, high resolution and minimized LER.

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Номер записи: 5
28-06-2012 дата публикации

Methods for producing bis(sulfonyl)imide ammonium salt, bis(sulfonyl)imide and bis(sulfonyl)imide lithium salt

Номер: US20120165571A1
Автор: Masao Iwaya, Ryuji Seki, Shouji Furuta
Принадлежит: Asahi Glass Co Ltd

To provide methods for producing a bis(sulfonyl)imide ammonium salt, a bis(sulfonyl)imide and a bis(sulfonyl)imide lithium salt simply and in good yield. A method for producing a bis(sulfonyl)imide ammonium salt, which comprises reacting a compound of the formula R—CHF—SO 2 X (wherein R is a C 1-4 fluorinated alkyl group which may contain an etheric oxygen atom, or a fluorine atom, and X is a fluorine atom or a chlorine atom) with ammonia in the absence of a catalyst. Further, methods for producing a bis(sulfonyl)imide and a bis(sulfonyl)imide lithium salt by using the bis(sulfonyl)imide ammonium salt.

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Номер записи: 6
03-01-2013 дата публикации

Preparation of 2,2-bis (fluoroalkyl) oxirane and preparation of photoacid generator therefrom

Номер: US20130005997A1
Автор: Koji Hasegawa, Masaki Ohashi, Masayoshi Sagehashi, Takeru Watanabe, Youichi Ohsawa
Принадлежит: Shin Etsu Chemical Co Ltd

A 2,2-bis(fluoroalkyl)oxirane (A) is prepared by reacting a fluorinated alcohol (1) with a chlorinating, brominating or sulfonylating agent under basic conditions to form an oxirane precursor (2) and subjecting the oxirane precursor to ring closure under basic conditions. R 1 and R 2 are fluoroalkyl groups, R 3 and R 4 are hydrogen or monovalent hydrocarbon groups, X is chlorine, bromine or —OSO 2 R 5 group, and R 5 is alkyl or aryl.

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Номер записи: 7
14-02-2013 дата публикации

Chemoselective enrichment for compound isolation

Номер: US20130041106A1
Автор: Antoinette Odendaal, Darci Trader, Erin E. Carlson
Принадлежит: Indiana University Research And Technology Corp

Chemoselective isolation of hydroxyl group-containing and carboxyl group-containing compounds is accomplished via formation of polymeric silyl ethers and polymeric siloxyl esters, respectively. Preparation of chemoselective polymeric reagents for capture of hydroxyl group containing compounds and carboxyl group containing compounds is described.

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Номер записи: 8
14-03-2013 дата публикации

Fluorine-Containing Sulfonate, Fluorine-Containing Sulfonate Resin, Resist Composition and Pattern Formation Method

Номер: US20130065182A1
Автор: Fumihiro Amemiya, Kazunori Mori, Masaki Fujiwara, Satoru Narizuka
Принадлежит: Central Glass Co Ltd

According to the present invention, there is provided a fluorine-containing sulfonate resin having a repeating unit of the following general formula (3). In order to prevent deficiency such as roughness after pattern formation or failure in pattern formation, the fluorine-containing sulfonate resin incorporates therein a photoacid generating function and serves as a resist resin in which “a moiety capable of changing its developer solubility by the action of an acid” and “a moiety having a photoacid generating function” are arranged with regularity.

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Номер записи: 9
14-03-2013 дата публикации

Method for manufacturing fluorine-containing imide compound

Номер: US20130066110A1
Автор: Noriaki Matsumura, Tsunetoshi Honda
Принадлежит: Mitsubishi Materials Corp

With this method for manufacturing fluorine-containing imide compounds, a method for manufacturing a fluorine-containing imide compound ((Rf 1 SO 2 )(Rf 2 SO 2 )NH) is selected which includes reaction of a fluorine-containing sulfonic acid (Rf 1 SO 3 H) and a fluorine-containing sulfonamide (Rf 2 SO 2 NH) in the presence of thionyl chloride. Wherein, Rf 1 and Rf 2 are fluorine, or straight-chain or branched perfluoroalkyl groups with a carbon number of 1-4.

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Номер записи: 10
21-03-2013 дата публикации

CRYSTALLINE FORMS OF A PURINE DERIVATIVE

Номер: US20130072504A1
Автор: Atherton Jonathan Charles Christian, Fernades Philippe, Northen Julian Scott, Skead Benjamin Mark, Worrall Christopher Peter
Принадлежит: CYCLACEL LIMITED

The present invention relates to new crystalline forms of a purine derivative which exhibits excellent anti-tumour activity. The invention also relates to a pharmaceutical composition containing said crystalline forms as an active ingredient, and use thereof in the prevention or treatment of disease. The invention further relates to a process for preparing the crystalline forms. 2. The crystalline form of which is a tartrate salt.3. The crystalline form of which is characterized by an x-ray powder diffraction pattern having two or more diffraction peaks at 2[theta] values selected from 6.67±0.2 claim 2 , 8.237±0.2 claim 2 , 9.777±0.2 claim 2 , 11.96±0.2 claim 2 , 12.38±0.2 claim 2 , 13.06±0.2 claim 2 , 13.38±0.2 claim 2 , 13.94±0.2 claim 2 , 14.90±0.2 claim 2 , 15.40±0.2 claim 2 , 15.95±0.2 claim 2 , 16.27±0.2 claim 2 , 16.54±0.2 claim 2 , 17.36±0.2 claim 2 , 17.57±0.2 claim 2 , 17.86±0.2 claim 2 , 19.64±0.2 claim 2 , 19.86±0.2 claim 2 , 20.12±0.2 claim 2 , 20.73±0.2 claim 2 , 21.14±0.2 claim 2 , 21.58±0.2 claim 2 , 22.57±0.2 claim 2 , 22.95±0.2 claim 2 , 23.29±0.2 claim 2 , 23.57±0.2 claim 2 , 24.07±0.2 claim 2 , 24.63±0.2 claim 2 , 25.30±0.2 claim 2 , 26.38±0.2 claim 2 , 27.09±0.2 claim 2 , 27.67±0.2 claim 2 , 27.97±0.2 claim 2 , 28.91±0.2 claim 2 , 29.28±0.2 claim 2 , 30.08±0.2 claim 2 , 30.41±0.2 claim 2 , 31.90±0.2 and 34.49±0.2 (Form E).45-. (canceled)6. The crystalline form of which is characterized by a differential scanning calorimetry trace recorded at a heating rate of 20° C. per minute which shows a maximum endothermic peak at a temperature between about 176° C. and about 185° C. claim 2 , or a differential scanning calorimetry trace substantially in accordance with that shown in .7. (canceled)8. The crystalline form of which is characterized by an x-ray powder diffraction pattern having two or more diffraction peaks at 2[theta] values selected from 3.82±0.2 claim 2 , 7.57±0.2 claim 2 , 8.12±0.2 claim 2 , 10.53±0.2 claim 2 , 11.39±0.2 claim 2 , 12.00±0.2 ...

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Номер записи: 11
18-04-2013 дата публикации

New Method of Using N-Thio Compounds for Oligonucleotide Synthesis

Номер: US20130096291A1
Автор: He Yigang, Mazur Wieslaw Adam, Sorokin Victor
Принадлежит: GIRINDUS AMERICA, INC.

A method for synthesizing an oligonucleotide which comprises using a sulfurizing agent of general formula (I) for sulfurizing at least one phosphorus internucleotide linkage of a precursor of the oligonucleotide, wherein R is an aryl group or a heteroaryl group, which is bonded to the S-atom through an annular carbon atom; and Rand Rare independently organic residues, preferably a C1-C20 hydrocarbon residue. The method may further comprise purifying the oligonucleotide. Also included is a process for the synthesis of the sulfurizing agent. 2. The method according to claim 1 , wherein R is a halophenyl or alkylphenyl claim 1 , Preferably 4-halophenyl claim 1 , especially preferably 4-chlorophenyl.3. The method according to any one of and wherein Rand Rare selected from lower alkyl or cycloalkyl (C1-C7) claim 1 , phenyl including substituted phenyl and naphthyl groups claim 1 , more preferably a methyl group.4. The method according to any one of to claim 1 , wherein the sulfurizing agent is dissolved in an organic solvent preferably a halogenated hydrocarbon solvent.5. The method according to any one of to claim 1 , wherein the molar ratio of sulfurizing agent to phosphorus internucleotide linkages to be sulfurized is from 1.0 to 2.0.6. The method according to any one of to claim 1 , wherein the precursor of said oligonucleotide contains nucleosides selected from ribonucleosides claim 1 , 2′-deoxyribonucleosides claim 1 , 2′-substituted ribonucleosides claim 1 , 2′-4′-locked-ribonucleosides claim 1 , 3′-amino-ribonucleosides claim 1 , 3′-amino-2′-deoxyribonucleosides.7. The method according to any one of to claim 1 , wherein the phosphorus internucleotide linkage is an H-phosphonate diester bond.8. The method according to claim 7 , wherein the coupling is carried out in solution phase.9. The method according to anyone of to which further comprises a step of purifying the oligonucleotide obtained according to anyone of to .10. The method according to which comprises at ...

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Номер записи: 12
02-05-2013 дата публикации

Process for converting natural oils to surfactants and biofuels

Номер: US20130109879A1
Автор: Christie H. Berger, Paul D. Berger
Принадлежит: OIL CHEM TECHNOLOGIES INC

A process for converting naturally occurring fats and oils to sulfonated surfactants that can be used in a variety of applications where surfactants are found to be applicable including but not restricted to Enhanced Oil Recovery, paper and pulp processing, mining, metal treating, adhesives, coatings, pesticide formulations, herbicide formulations, fungicide formulations. The byproduct of such a process is a useful solvent or source of biodiesel fuel.

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Номер записи: 13
16-05-2013 дата публикации

POLYMORPHIC FORMS OF LAPATINIB DITOSYLATE AND PROCESSES FOR THEIR PREPARATION

Номер: US20130123497A1
Автор: Cammisa Eduardo Gustavo, Weeratunga Gamini, Zetina-Rocha Carlos
Принадлежит: APOTEX PHARMACHEM INC.

There is provided a crystalline form of Lapatinib, termed APO-I, and methods for making APO-I. There is also provided a crystalline solvate form of Lapatinib, termed APO-II, and methods for making APO-II. 1. APO-I polymorphic form of Lapatinib ditosylate.2. The APO-I polymorphic form of Lapatinib ditosylate of having a powder X-ray diffraction pattern comprising peaks claim 1 , in terms of degrees 2-theta claim 1 , at approximately 4.6 claim 1 , 18.8 claim 1 , 19.5 claim 1 , 21.3 claim 1 , 22.0 and 23.0.3. The APO-I polymorphic form of Lapatinib ditosylate of wherein the powder X-ray diffraction pattern further comprising peaks claim 2 , in terms of degrees 2-theta claim 2 , at approximately 8.3 claim 2 , 9.3 claim 2 , 11.8 claim 2 , 13.8 claim 2 , 14.9 claim 2 , 16.8 claim 2 , 17.3 claim 2 , 25.2 and 26.2.4. The APO-I polymorphic form of Lapatinib ditosylate of having a DSC thermogram comprising two endothermic peaks with peak onset temperatures of approximately 169.5° C. and 247.9° C. and peak maximums of approximately 179.5° C. and 250.5° C.5. The APO-I polymorphic form of Lapatinib ditosylate of having a PXRD diffractogram substantially similar to a PXRD diffractogram as depicted in .6. The APO-I polymorphic form of Lapatinib ditosylate of having a DSC thermogram substantially similar to a DSC thermogram as depicted in .7. APO-II polymorphic form of Lapatinib ditosylate.8. The APO-II polymorphic form of Lapatinib ditosylate of having a powder X-ray diffraction pattern comprising peaks claim 7 , in terms of degrees 2-theta claim 7 , at approximately 4.4 claim 7 , 8.3 claim 7 , 13.1 claim 7 , 19.3 claim 7 , 20.9 and 21.4.9. The APO-II polymorphic form of Lapatinib ditosylate of wherein the powder X-ray diffraction pattern further comprising peaks claim 8 , in terms of degrees 2-theta claim 8 , at approximately 9.6 claim 8 , 10.5 claim 8 , 14.0 claim 8 , 15.0 16.9 claim 8 , 18.2 claim 8 , 25.3 claim 8 , and 26.6.10. The APO-II polymorphic form of Lapatinib ...

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Номер записи: 14
30-05-2013 дата публикации

PROCESS FOR PREPARING AND PURIFYING SALTS OF ACRYLAMIDO-2-METHYLPROPANESULFONIC ACID

Номер: US20130137893A1
Автор: Bartling Karsten, Ebel Klaus, Keller Andreas, LANGLOTZ Björn, Rüdenauer Stefan, Steiner Jochen, Voitl Tobias
Принадлежит: BASF SE

A process for preparing salts of acrylamido-2-methylpropanesulfonic acid (A) using the steps of: 1. A process for preparing salts of acrylamido-2-methylpropanesulfonic acid (A) comprising the steps of: [{'br': None, 'sup': a', 'b', 'c, 'NRRR\u2003\u2003(I)'}, {'sup': a', 'b', 'c, 'where the R, Rand Rradicals are each independently, {'sub': 1', '4', '1', '4', '1', '4, 'hydrogen, C-C-alkyl, hydroxy-C-C-alkyl or C-C-alkoxy,'}, 'where the molar ratio of compound (A) to the basic component (B) is preferably 1:1 to 1:3,, 'a) preparing a solution of a contaminated salt of acrylamido-2-methylpropanesulfonic acid (A) in an anhydrous organic solvent (L) using at least one basic component (B) selected from the group of alkali metal oxides, alkaline earth metal oxides, alkali metal hydroxides, alkaline earth metal hydroxides and amines of the general formula (I)'}b) optionally partly removing the organic solvent (L) at a pressure in the range from 0.001 to 2 bar (abs),c) recovering the dissolved salt of compound (A) by crystallization or by precipitation, by altering the temperature and/or the pressure and/or the concentration of the salt in the solution,d) optionally drying the purified salt of acrylamido-2-methylpropanesulfonic acid (A).2. The process according to claim 1 , wherein the anhydrous solvent (L) used is a solvent from the group of: methanol claim 1 , ethanol claim 1 , propanol claim 1 , butanol claim 1 , acetonitrile claim 1 , acetone claim 1 , DMF claim 1 , or a mixture of at least two of these solvents.3. The process according to claim 1 , wherein claim 1 , in step a) claim 1 , an alkali metal salt of acrylamido-2-methylpropanesulfonic acid is used.4. The process according to claim 1 , wherein claim 1 , in step a) claim 1 , a salt of acrylamido-2-methylpropanesulfonic acid (A) with an amine of the formula (I) is used.5. The process according to claim 1 , wherein claim 1 , in step b) claim 1 , at least 50% by weight of the organic solvent (L) is removed at a ...

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Номер записи: 15
30-05-2013 дата публикации

PROCESS FOR PRODUCING FLUORINE-CONTAINING SULFONYLIMIDE COMPOUND

Номер: US20130137899A1
Автор: Honda Tsunetoshi, Takano Daisuke
Принадлежит:

In this process for producing a fluorine-containing sulfonylimide compound, a process for producing a fluorine-containing sulfonylimide compound ((RfSO)(RfSO)N.M) is employed that comprises a first step of obtaining a reaction liquid by reacting a perfluoroalkylsulfonyl fluoride (RfSOF) with ammonia, a second step of obtaining a mixture containing an alkaline metal salt of a perfluoroalkylsulfonamide (Rf'SONH.M) by reacting the reaction liquid with at least one type of alkaline metal compound selected from among hydroxides, carbonates and bicarbonates of alkaline metals M of either Li, Na or K, and a third step of reacting the mixture with a perfluoroalkylsulfonyl halide (RfSOX), wherein Rfand Rfrepresent linear or branched perfluoroalkyl groups having 1 to 4 carbon atoms, and X represents fluorine or chlorine. 3. The process for producing a fluorine-containing sulfonylimide compound according to claim 1 , wherein claim 1 ,in the first step, the ammonia is aqueous ammonia and the resulting reaction liquid is an aqueous solution, andin the second step, the reaction between the reaction liquid and the alkaline metal compound is carried out in the aqueous solution.4. The process for producing a fluorine-containing sulfonylimide compound according to claim 1 , further comprising a fourth step of recovering ammonia generated in the second step and supplying to the first step.5. The process for producing a fluorine-containing sulfonylimide compound according to claim 1 , wherein the concentration of the aqueous ammonia is within the range of 1% to 50%.6. The process for producing a fluorine-containing sulfonylimide compound according to claim 1 , wherein the molar amount of the aqueous ammonia is within the range of 3 to 20 times that of the perfluoroalkylsulfonyl fluoride.7. The process for producing a fluorine-containing sulfonylimide compound according to claim 1 , wherein the temperature of the reaction between the perfluoroalkylsulfonyl fluoride and the aqueous ...

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Номер записи: 16
13-06-2013 дата публикации

COMPOSITIONS, METHODS, AND SYSTEMS FOR THE SYNTHESIS AND USE OF IMAGING AGENTS

Номер: US20130149244A1
Автор: Benites Pedro, Cesati Richard R., Cheesman Edward H., Lazewatsky Joel, Lee L. Veronica, Looby Richard J., Purohit Ajay, Radeke Heike S.
Принадлежит: Lantheus Medical Imaging, Inc.

The present invention generally relates to novel synthetic methods, systems, kits, salts, and precursors useful in medical imaging. In some embodiments, the present invention provides compositions comprising an imaging agent precursor, which may be formed using the synthetic methods described herein. An imaging agent may be converted to an imaging agent using the methods described herein. In some cases, the imaging agent is enriched in F. In some cases, an imaging agent including salt forms (e.g., ascorbate salt) may be used to image an area of interest in a subject, including, but not limited to, the heart, cardiovascular system, cardiac vessels, brain, and other organs. 4. The composition of claim 3 , wherein X is halide claim 3 , phosphate claim 3 , sulfate claim 3 , trifluoroacetate claim 3 , toluenesulfonate claim 3 , acetate claim 3 , formate claim 3 , citric claim 3 , ascorbate claim 3 , mesylate (methanesulfonate) claim 3 , or benzoate.6. The composition of claim 1 , wherein at least one Ris not hydrogen.921-. (canceled)24. (canceled)2648-. (canceled)49. The method of any one of claims 23 , wherein the step of reacting comprises exposing a compound comprising formula (II) or (IV) to a source of fluoride.50. The method of claim 49 , wherein the source of fluoride is isotopically enriched with F.5158-. (canceled)60. (canceled)62. (canceled)63. The salt of claim 61 , wherein the fluorine is isotopically enriched with F.64. A pharmaceutically acceptable composition comprising a salt of claim 63 , and optionally a pharmaceutically acceptable excipient.65. A kit comprising a salt of and instructions for use66. A method of imaging a subject claim 63 , comprising:{'claim-ref': {'@idref': 'CLM-00063', 'claim 63'}, 'administering a dose of a pharmaceutically acceptable composition comprising a salt of and optionally a pharmaceutically acceptable excipient, to a subject; and'}acquiring at least one image of a portion of the subject.6768-. (canceled)70. The method of ...

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Номер записи: 17
13-06-2013 дата публикации

PROCESS FOR THE MANUFACTURE OF CHIRAL CATALYSTS AND THEIR SALTS

Номер: US20130150574A1
Автор: Henschke Julian Paul, Wu Ping-Yu
Принадлежит: ScinoPharm Taiwan, Ltd.

The present invention provides efficient and economical methods for synthesis of (−)-2-exo-morpholinoisoborne-10-thiol, its enantiomer, and related chiral catalysts. Novel compounds and methods of asymmetric synthesis are also disclosed. 2. A process according to claim 1 , wherein the first reducing agent is an aluminum hydride reagent.3. A process according to claim 2 , wherein the aluminum hydride reagent is sodium bis(2-methoxyethoxy)aluminum hydride.4. A process according to claim 1 , wherein the second reducing agent is selected from the group consisting of a metal including zerovalent metals claim 1 , zerovalent metal alloys claim 1 , and non-zerovalent metals claim 1 , a metal hydride and a highly reactive thiol.5. A process according to claim 1 , wherein R claim 1 , R claim 1 , and N together form a morpholine group.8. A process according to claim 7 , wherein the compound of formula (Is) is the exo-diastereomer.9. A process according to claim 7 , wherein the acid is HCl.11. A compound according to claim 10 , wherein HX is HCl.1716. A method of asymmetric synthesis comprising contacting a compound according to any one of - with reactants in an asymmetric transformation to stereoselectively provide a product.18. The method according to claim 17 , wherein the asymmetric transformation is an asymmetric addition reaction. This application claims the benefit of priority to U.S. Provisional Application Ser. No. 61/565,449, filed Nov. 30, 2011, the entire content of which is incorporated herein by reference.NOT APPLICABLENOT APPLICABLE((−)-2-exo-morpholinoisoborne-10-thiol, abbreviated as “(−)-MITH” and classified as a γ-aminothiol ligand, is an efficient catalyst that induces the stereoselective formation of chiral carbon centers in certain reactions (2006, 71, 833-835). (−)-MITH (CAS No. 874896-16-9) has the systematic name ((1R,2R,4R)-7,7-dimethyl-2-morpholino-bicyclo[2.2.1]heptan-1-yl)methanethiol and the structure:The abbreviation MITH is used herein to apply ...

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Номер записи: 18
20-06-2013 дата публикации

PROCESS FOR THE MANUFACTURE OF DABIGATRAN ETEXILATE

Номер: US20130158270A1
Автор: DACH Rolf, GNAD Frieder, HEDDESHEIMER Ingo, HEITGER Helmut, MEINECK Seigfried, MUELLER-BOETTICHER Hermann, Schmitt Stefan
Принадлежит: BOEHRINGER INGELHEIM INTERNATIONAL GMBH

An improved process for preparing dabigatran etexilate, as well as analogous compounds of formula 7, 110-. (canceled)14. The compound according to claim 13 , wherein Ris n-hexyl.16. The compound according to claim 15 , wherein Ris methyl claim 15 , Ris ethyl and Hal is chlorine. Substituted (4-benzimidazol-2-ylmethylamino)-benzamidines, particularly dabigatran etexilate (CAS 593282-20-3), are already known from International Patent Application WO 98/37075 as active substances with a thrombin-inhibiting and thrombin time-prolonging activity. The main indication sectors of the compound of chemical formula I are the postoperative prophylaxis of deep vein thromboses and stroke prevention (prevention of stroke due to atrial fibrillation, SPAF for short).In WO 98/37075 it is proposed to produce the substituted (4-benzimidazol-2-ylmethyl-amino)-benzamidines by reacting corresponding substituted (4-benzimidazol-2-ylmethylamino)-benzonitriles with ammonia. This process is extremely onerous from the manufacturing point of view and results in a large quantity of acids that have to be disposed of (cf. also WO 2007/071743, WO 2007/ 071742).An improved process for preparing dabigatran etexilate and analogous compounds thereof is described hereinafter. By switching to new starting materials, the use of phase transfer catalysis and the formation of the benzimidazole without the use of coupling reagents a significantly more efficient synthesis of dabigatran etexilate is achieved. The high selectivity in the coupling of the intermediates (step 2) contributes significantly to the economy of the new synthesis route.The present invention describes a process for preparing compounds of formula 7:wherein R, Rand Rhere and hereinafter each independently of one another denote C-alkyl and Hal=chlorine or bromine, preferably chlorine, according to the invention haloacetic acid anhydride 5b-1, haloacetic acid 5b-2, ortho-haloacetate 5b-3 or haloacetyl chloride 5b-4 may be used for 5, and ...

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Номер записи: 19
27-06-2013 дата публикации

AMINE ADDUCTS, DERIVATIVES THEREOF, METHODS FOR MAKING SUCH ADDUCTS AND DERIVATIVES, AND METHODS FOR USING SUCH ADDUCTS AND DERIVATIVES

Номер: US20130161014A1
Автор: Degre Guillaume, Morvan Mikal, Pakenham Derek
Принадлежит: Rhodia Operations

An amine adduct is made by (1) forming an addition intermediate by heating a mixture comprising at least one diene and at least one unsaturated fatty acyl compound, and reacting the addition intermediate with a diamine to form the amine adduct, or by (2) reacting at least one unsaturated fatty acyl compound with at least one diamine to form an amine intermediate, and heating a mixture of the amidoamine intermediate and at least one diene to form the amine adduct, or by (3) reacting at least one unsaturated fatty tertiary amine compound with at least at least one diene to form the amine adduct. A surfactant composition is derived from the amine adduct and is particularly useful in a method for enhancing the recovery of oil from a reservoir having a production wellbore, comprising introducing an aqueous flooding fluid into the reservoir at one or more locations different from the location of the production wellbore, said fluid comprising the surfactant composition and recovering the oil through the production wellbore. 1. An amine adduct , comprising the product obtained by: '(b) reacting the addition intermediate with a diamine to form the amine adduct, or', '(1)(a) forming an addition intermediate by heating a mixture comprising at least one diene and at least one unsaturated fatty acyl compound, and'} '(b) heating a mixture of the amidoamine intermediate and at least one diene to form the amine adduct, or', '(2)(a) reacting at least one unsaturated fatty acyl compound with at least one diamine to form an amidoamine intermediate, and'}(3) reacting at least one unsaturated fatty tertiary amine compound with at least at least one diene to form the amine adduct.2. The amine adduct of wherein the adduct is an amidoamine product claim 1 , obtained by: '(b) reacting the addition intermediate with a diamine to form the amidoamine product, or', '(1)(a) forming an addition intermediate by heating a mixture comprising at least one diene and at least one unsaturated fatty acyl ...

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Номер записи: 20
27-06-2013 дата публикации

PROCESSES FOR PREPARING PEMETREXED

Номер: US20130165654A1
Автор: Gunda Nageshwar, Kadaboina Rajasekhar, Manda Amarendhar, Murki Veerender, Nariyam Sekhar Munaswamy, Vinjamuri Raghupati Rama
Принадлежит:

The present invention relates to pemetrexed disodium substantially free from specific process-related impurities, and processes for the preparation thereof. 3. The process according to claim 1 , wherein step a) is carried out in the presence of a coupling agent and a base.4. The process according to claim 3 , wherein a coupling agent is 2-chloro-4 claim 3 ,6-dimethoxy-1 claim 3 ,3 claim 3 ,5-triazine claim 3 , isobutyl chloroformate claim 3 , dicyclohexylcarbodiimide and 1-hydroxybenzotriazole claim 3 , 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide claim 3 , or its hydrochloride and 1-hydroxybenzotriazole.5. The process according to claim 3 , wherein the base is N-methyl morpholine or triethylamine.6. The process according to claim 3 , wherein a coupling agent is 2-chloro-4 claim 3 ,6-dimethoxy-1 claim 3 ,3 claim 3 ,5-triazine and a base is N-methylmorpholine.7. The process according to claim 1 , wherein the reaction of step a) is conducted at temperatures about 0° C. to about 50° C.16. (canceled) The present application relates to processes for preparing pemetrexed and its salts.A chemical name for the drug compound “pemetrexed” is 2-[4-[2-(4-amino-2-oxo-3,5,7-triazabicyclo[4.3.0]nona-3,8,10-trien-9-yl)ethyl]benzoyl]amino-pentanedioic acid. The drug compound having the adopted name “pemetrexed disodium” is also known by the chemical name L-glutamic acid, N-[4-[2-(2-amino-4,7-dihydro-4-oxo-1H-pyrrolo[2,3-d]pyrimidin-5-yl)ethyl]benzoyl]-disodium salt, heptahydrate, and is represented by the structure of Formula I.Pemetrexed is an anti-folate anti-neoplastic agent that exerts its action by disrupting folate-dependent metabolic processes essential for cell replication. It is believed to work by inhibiting three enzymes that are required in purine and pyrimidine biosynthesis-thymidylate synthase (TS), dihydrofolate reductase (DHFR), and glycinamide ribonucleotide formyl transferase (GARFT). Pemetrexed disodium heptahydrate is the active ingredient in a lyophilized ...

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Номер записи: 21
04-07-2013 дата публикации

Surface Active Agents Derived from Biodiesel-Based Alkylated Aromatic Compounds

Номер: US20130172589A1
Автор: Daniel R. Weaver, George A. Smith, Zheng Chai
Принадлежит: Huntsman Petrochemical LLC

A surface active agent comprising an arylated methyl ester of a fatty acid, or mixture of fatty acids, derived from biodiesel or a triglyceride source is disclosed. The fatty acid mixture is condensed to methyl esters and alkylated with aromatic substituents under Friedel-Crafts conditions. The alkylated methyl esters may be alkoxylated using a catalyst derived from fatty acids, alkaline earth salts, and strong acids. The resulting nonionic surfactant may also be sulfonated to produce one class of anionic surfactants. The alkylated methyl esters may also be directly sulfonated to produce another class of anionic surfactants.

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Номер записи: 22
11-07-2013 дата публикации

SULFONIC ACID GROUP-CONTAINING DIAMINE COMPOUND AND METHOD FOR PRODUCING THE SAME

Номер: US20130178649A1
Автор: Sugitani Tooru
Принадлежит: NITTO DENKO CORPORATION

The present invention provides a novel sulfonic acid group-containing diamine compound represented by formula (1) below, and a method for producing the same. This compound has a fluorene skeleton with sulfonic acid groups or derivatives thereof. In this compound, a substituent having an amino group is bonded to each of carbon atoms at the 2-position and the 7-position in the skeleton, and no substituent is bonded to a carbon atom at the 9-position in the skeleton. A in formula (1) denotes an optionally-substituted divalent aliphatic group (having a carbon number of 10 or less) or an optionally-substituted divalent aromatic group (having the number of rings of 4 or less), for example. The present invention relates to a novel sulfonic acid group-containing diamine compound having amino groups and a fluorene skeleton with sulfonic acid groups, and to a method for producing the compound.Diamine compounds having sulfonic acid groups or derivatives of sulfonic acid group (sulfonic acid group-containing diamine compounds) are widely used as a crosslinking agent or a raw material for thermosetting polymers or polycondensation polymers such as polyamide, polyimide, epoxy resin, and polyurethane. Fluorene has a fused ring structure composed of three rings, and has a high planarity of the molecular structure. Polymers formed using a sulfonic acid group-containing diamine compound having a fluorene skeleton as a raw material or a crosslinking agent are expected to have properties derived from the high planarity of the fluorene skeleton.The carbon atom located at the 9-position in the fluorene skeleton is a carbon atom of methylene group, and it thus has a higher reactivity compared to other carbon atoms in the skeleton. Therefore, conventionally, a number of sulfonic acid group-containing diamine compounds (see Patent Literature 1) in which a substituent having an amino group is bonded to the carbon atom at the 9-position in the skeleton, such as 9,9-bis(3,5-dimethyl-4- ...

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Номер записи: 23
25-07-2013 дата публикации

PROCESSES FOR THE PREPARATION OF 4'-[3-[4-(6-FLUORO-1,2-BENZISOXAZOL-3-YL)PIPERIDINO]PROPOXY]-3'-METHOXYACETOPHENONE AND INTERMEDIATES THEREOF

Номер: US20130190501A1
Автор: Krishna Reddy Pingili, Mohan Rao Dodda, Venkat Reddy Buthukuri
Принадлежит: SYMED LABS LIMITED

The present invention relates to processes for the preparation of 4′-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidino]propoxy]-3′-methoxyacetophenone and intermediates thereof. The present invention also provides a process for purifying 4′-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidino]propoxy]-3′-methoxyacetophenone to obtain the purity greater than about 98.0 area % to about 99.0 area % as measured by HPLC, preferably greater than about 99.0 area % to about 99.5 area %, more preferably greater about 99.5 area % to about 99.9 area %. individual impurities lower than about 0.15 area %, preferably lower than about 0.1% and total impurities lower than about 0.5 area % by HPLC. 130-. (canceled)32. A process of claim 31 , wherein the oxidizing agent is selected from the group consisting of collin's reagent claim 31 , pyridinium dichromate claim 31 , pyridinium chlorochromate claim 31 , pyridinium chlorochromate on alumina claim 31 , DMSO-DCC claim 31 , DMSO-acetic anhydride or mixtures thereof claim 31 , preferably DMSO-DCC or DMSO-acetic anhydride.33. A process of claim 31 , wherein the solvent used optionally is selected from the group consisting of water claim 31 , halogenated solvents like dichloromethane claim 31 , ethylene dichloride claim 31 , chloroform claim 31 , chlorobenzene claim 31 , esters like ethyl acetate claim 31 , isopropyl acetate claim 31 , tertiary butyl acetate hydrocarbon solvents like n-heptane claim 31 , cyclohexane claim 31 , n-hexane claim 31 , toluene claim 31 , xylene claim 31 , ethers like tetrahydrofuran claim 31 , 1 claim 31 ,4-dioxane claim 31 , aprotic polar solvents like N claim 31 ,N-dimethylformamide (DMF) claim 31 , dimethylsulfoxide (DMSO) claim 31 , N claim 31 ,N-dimethylacetamide (DMA) claim 31 , N-methyl pyrrlolidine (NMP) or mixtures thereof claim 31 , preferably water or halogenated solvent.34. The process of claim 31 , wherein the reaction is carried out optionally in the presence of an acid.36. A process of claim 35 , ...

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Номер записи: 24
01-08-2013 дата публикации

PROCESSES FOR THE PREPARATION OF FESOTERODINE

Номер: US20130197260A1
Автор: DWIVEDI Shriprakash Dhar, JAIN Kuldeep Natwarlal, PRASAD Ashok
Принадлежит: CADILA HEALTHCARE LIMITED

The invention relates to improved process for the preparation of fesoterodine and its pharmaceutically acceptable salt, specifically fesoterodine fumarate of formula (1). The invention relates to solid state forms of a novel salt of fesoterodine and process for the preparation thereof. The invention also relates to highly pure fesoterodine fumarate substantially free of impurity X at RRT 1.37. The invention also provides solid particles of pure fesoterodine fumarate wherein 90 volume-percent of the particles (D90) have a size of higher than 200 microns. 1. Fesoterodine 2-chloro-mandelate.2. The fesoterodine 2-chloro-mandelate as claimed in claim 1 , which is in a crystalline form or an amorphous form.3. The fesoterodine 2-chloro-mandelate as claimed in claim 1 , wherein 2-chloro-mandelic acid is racemic(±) 2-chloro-mandelic acid claim 1 , S-(+)-2-chloro-mandelic acid claim 1 , or R-(−)-2-chloro-mandelic acid.4. The festerodine 2-chloro mandelate as claimed in claim 3 , wherein the 2-chloro-mandelic acid is S-(+)-2-chloro-mandelic acid.5. Fesoterodine 2-chloro-mandelate as claimed in claim 1 , with one or more of the following properties:i) a powder X-ray diffraction pattern having peaks at about 9.9, 12.9, 14.2, 19.2, 20.7 and 24.9±0.2 degrees 2-theta;{'figref': {'@idref': 'DRAWINGS', 'FIG. 5'}, 'ii) a powder X-ray diffraction pattern as depicted in ;'}{'figref': {'@idref': 'DRAWINGS', 'FIG. 6'}, 'iii) a DSC thermogram having an endotherm peak at about 162° C. or substantially as depicted in ; or'}{'sup': '−1', 'figref': {'@idref': 'DRAWINGS', 'FIG. 7'}, 'iv) an infrared spectrum having absorption bands at about 3346, 2985, 2970, 2939, 2873, 2603, 2368, 1755, 1620, 1492, 1388, 1328, 1224, 1190, 1120, 1087, 1062, 1031, 970, 916, 867, 819, 759, 732, 705, 607, 582. 561, 522 and 501 cmor a spectrum depicted in .'}6. A process for the preparation of fesoterodine 2-chloro-mandelate claim 1 , the process comprising obtaining a solution of fesoterodine in one or more ...

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Номер записи: 25
08-08-2013 дата публикации

POLYGLYCOL ETHER-FREE SULPHOSUCCINATES BASED ON POLYGLYCEROL PARTIAL ESTERS AND USE THEREOF

Номер: US20130204021A1
Автор: Berkels Wolfgang, Hartung Christian, Herrwerth Sascha, Klein Ralf, Muss Peter, Peggau Joerg, Schuch Dominik, Springer Oliver, Wenk Hans Henning, Westerholt Ursula
Принадлежит: Evonik Industries AG

The invention relates to polyglycol ether-free, polyglycerol partial ester-based sulphosuccinates, the preparation thereof, and the use of these in cosmetic formulations and also in cleaning compositions in the industrial and domestic sector and formulations comprising these sulphosuccinates. 2. The sulphosuccinate according to claim 1 , wherein R claim 1 , R claim 1 , R═H and wherein on statistical average claim 1 , said sulphosuccinate has a weight ratio of carboxylic acid ROH to polyglycerol basic backbone of 0.10:1 to 0.50:1.3. The sulphosuccinate according to claim 1 , wherein said sulphosuccinate has an average degree of polymerization n of 2 to 11.4. The sulphosuccinate according to claim 1 , wherein R=an acyl radical of a fatty acid selected from the group consisting of oenanthic acid claim 1 , caprylic acid claim 1 , pelargonic acid claim 1 , capric acid claim 1 , lauric acid claim 1 , myristic acid claim 1 , pentadecanoic acid claim 1 , palmitic acid claim 1 , margaric acid claim 1 , stearic acid claim 1 , undecylenic acid claim 1 , myristoleic acid claim 1 , palmitoleic acid claim 1 , petroselic acid claim 1 , oleic acid claim 1 , elaidic acid claim 1 , vaccenic acid claim 1 , linoleic acid claim 1 , α-linolenic acid claim 1 , γ-linolenic acid claim 1 , calendic acid claim 1 , punicic acid claim 1 , α-elaeostearic acid claim 1 , β-elaeostearic acid claim 1 , and mixtures thereof.5. The sulphosuccinate according to claim 1 , wherein R is selected from sulphosuccinic acid radicals of the formula IIa or IIb.6. The sulphosuccinates according to claim 1 , wherein Ris selected from sulphomethylsuccinic acid radicals of the formula IIc or IId.7. The sulphosuccinate according to claim 1 , wherein R=the acyl radical of a natural fatty acid selected from the group consisting of caprylic acid claim 1 , capric acid claim 1 , lauric acid claim 1 , and coconut fatty acid mixtures and Ris selected from sulphosuccinic acid radicals of the formula IIa or IIb.8. A process ...

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Номер записи: 26
15-08-2013 дата публикации

SALTS OF 5-SULFOISOPHTHALIC ACID AND METHOD OF MAKING SAME

Номер: US20130211116A1
Автор: OSTER Timothy A.
Принадлежит:

This invention relates to methods for the production of various metal salts of 5-sulfoisophthalic acid including those where the metal cation is selected from the group consisting of silver (I), sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, barium, manganese (II), iron (II), cobalt (II), nickel (II), copper (I), copper (II), zinc, yttrium, and cadmium. The methods utilize a solvent system that comprises acetic acid or water or a mixture of both. The invention also encompasses the various metal salts of 5-sulfoisophthalic acid. 1. A process for the preparation of metal salts of 5-sulfoisophthalic acid , the process comprising the steps of:forming a solvent system comprising 5-sulfoisophthalic acid, a metal cation producing compound, and acetic acid and water wherein the acetic acid to water ratio is between and includes 0:1 and 1:0 and wherein said metal cation is selected from the group consisting of silver (I), sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, barium, manganese (II), iron (II), cobalt (II), nickel (II), copper (I), copper (II), zinc, yttrium, and cadmium; andmaintaining said solvent system under conditions sufficient to form a metal salt of 5-sulfoisophthalic acid.2. A process according to wherein said solvent system comprises acetic acid and water.3. A process according to wherein said metal cation producing compound comprises a metal salt.4. A process according to further comprising the prior step of isolating 5-sulfoisphthalic acid from a sulfonation solution and washing said 5-sulfoisophthalic acid prior to forming said solvent system.5. A process according to further comprising the steps of recovery of said metal salt of 5-sulfoisophthalic acid and recycle of said solvent system.6. A process according to wherein said metal cation is selected from the group consisting of sodium claim 1 , potassium claim 1 , and rubidium.7. A process according to wherein said metal cation is cesium.8. A process according ...

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Номер записи: 27
15-08-2013 дата публикации

USE OF AN ACETIC ACID WASH TO PREPARE LOW-SULFATE 5-SULFOISOPHTHALIC ACID, MONO-LITHIUM SALT

Номер: US20130211120A1
Автор: Coleman Michael Todd, OSTER Timothy A.
Принадлежит: FUTURE FUEL CHEMICAL COMPANY

There is disclosed a process for making a mono-lithium salt of 5-sulfoisophthalic acid (LiSIPA) having less than 500 ppm sulfate. The process uses a reaction mixture of water, a lithium cation producing compound, and 5-sulfoisophthalic acid. The reaction mixture is heated to reflux, cooled, filtered and washed with acetic acid to obtain a high quality LiSIPA having less than 500 ppm sulfate. Also disclosed is a high quality, non-purified reaction product containing a mono-lithium salt of 5-sulfoisophthalic acid and having less than 500 ppm sulfate. 1. A process for the preparation of a low sulfate , lithium salt of 5-sulfoisophthalic acid , the process comprising the steps ofdrowning a solution of 5-sulfoisophthalic acid into a solution consisting essentially of a lithium cation producing compound and water to form a reaction mixture;maintaining the reaction mixture under conditions sufficient to form a lithium salt of 5-sulfoisophthalic acid;isolating said lithium salt of 5-sulfoisophthalic acid from the reaction mixture; andwashing said isolated lithium salt of 5-sulfoisophthalic acid with acetic acid.2. A process according to further comprising the prior step of forming 5-sulfoisophthalic acid from isophthalic acid and a sulfur containing compound.3. A process according to wherein said lithium cation producing compound is selected from the group consisting of lithium hydroxide monohydrate claim 1 , anhydrous lithium hydroxide claim 1 , organic lithium salts claim 1 , and inorganic lithium salts.4. A process according to wherein the lithium compound is lithium hydroxide monohydrate.5. A process according to where the organic lithium salt is lithium acetate and the inorganic lithium salt is selected from the group consisting of lithium carbonate and lithium bicarbonate.6. A process according to wherein the mole ratio of lithium cation to 5-sulfoisophthalic acid is at least 0.95:1.7. A process according to wherein the step of maintaining the reaction mixture ...

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Номер записи: 28
15-08-2013 дата публикации

PROCESS FOR PRODUCING OPTICALLY ACTIVE BETA-AMINO ALDEHYDE COMPOUND

Номер: US20130211139A1
Автор: Hayashi Yujiro
Принадлежит: Sumitomo Chemical Company, Limited

The invention relates to a method of producing optically active β-aminoaldehyde compound (3) by reacting imine compound (1-1) or sulfone compound (1-2) with aldehyde compound (2) in the presence of an optically active pyrrolidine compound.

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Номер записи: 29
22-08-2013 дата публикации

PHOSPHINE LIGANDS FOR CATALYTIC REACTIONS

Номер: US20130217876A1
Автор: BARNES David M., Chan Vincent S., Dunn Travis B., Franczyk Thaddeus S., Haight Anthony R., Shekhar Shashank
Принадлежит: AbbVie Inc.

The disclosure is directed to: (a) phosphacycle ligands; (b) catalyst compositions comprising phosphacycle ligands; and (c) methods of using such phosphacycle ligands and catalyst compositions in bond forming reactions. 2. The phosphine ligand of claim 1 , wherein Vand Vare CR claim 1 , wherein Ris alkoxy.3. The phosphine ligand of claim 1 , wherein Vand Vare CR claim 1 , wherein Ris methoxy.4. The phosphine ligand of claim 1 , wherein Vand Vare CR claim 1 , wherein Ris hydrogen.5. The phosphine ligand of claim 1 , wherein V claim 1 , Vand Vare CR claim 1 , wherein Ris alkyl.6. The phosphine ligand of claim 1 , wherein V claim 1 , Vand Vare CR claim 1 , wherein Ris isopropyl.7. The phosphine ligand of claim 1 , wherein Vand Vare CR claim 1 , wherein Ris hydrogen.10. The phosphine ligand of claim 1 , wherein the ligand is selected from the group consisting of:2,2,6,6-tetramethyl-1-(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphinane;2,2,6,6-tetramethyl-1-(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphinan-4-one;2,2,6,6-tetramethyl-1-(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphinan-4-ol;7,7,9,9-tetramethyl-8-(2′,4′,6′-triisopropylbiphenyl-2-yl)-1,4-dioxa-8-phosphaspiro[4.5]decane;8,8,10,10-tetramethyl-9-(2′,4′,6′-triisopropylbiphenyl-2-yl)-1,5-dioxa-9-phosphaspiro[5.5]undecane;3,3,8,8,10,10-hexamethyl-9-(2′,4′,6′-triisopropylbiphenyl-2-yl)-1,5-dioxa-9-phosphaspiro[5.5]undecane;1-(2′-(dimethylamino)-6′-methoxybiphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′,6′-bis(dimethylamino)biphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′,6′-dimethoxybiphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′,6′-diisopropoxybiphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′-(dimethylamino)biphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(biphenyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(1,1′-binaphthyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(2′-methoxy-1,1′-binaphthyl-2-yl)-2,2,6,6-tetramethylphosphinan-4-one;1-(3,6-dimethoxybiphenyl-2-yl)-2,2,6,6- ...

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Номер записи: 30
29-08-2013 дата публикации

SULFONATES FROM NATURAL OIL METATHESIS

Номер: US20130225473A1
Автор: Allen Dave R, Bernhardt Randal J, Brown Aaron, Luebke Gary, Luka Renee, Malec Andrew D., Masters Ronald A., Skelton Patti, Sook Brian, Weitgenant Jeremy Aaron, Wolfe Patrick Shane
Принадлежит: STEPAN COMPANY

Sulfonate compositions are disclosed. The compositions include alkanesulfonates, alkenesulfonates, sultones, and hydroxy-substituted alkanesulfonates. The sulfonates comprise a reaction product of a metathesis-derived C10-C17 monounsaturated acid, octadecene-1,18-dioic acid, or their ester derivatives with a sulfonating or sulfitating agent. In one aspect, the sulfonate composition is a sulfo-estolide made by reacting a metathesis-derived C10-C17 monounsaturated acid or octadecene-1,18-dioic acid with a sulfonating agent, optionally in the presence of a saturated fatty acid. The sulfonates are valuable for a wide variety of end uses, including cleaners, fabric treatment, hair conditioning, personal care (liquid cleansing products, conditioning bars, oral care products), paint additives, antimicrobial compositions, agricultural uses, and oil field applications. 1. A sulfonate composition comprising a reaction product of a metathesis-derived C-Cmonounsaturated acid , octadecene-1 ,18-dioic acid , or their ester derivatives with a sulfonating or sulfitating agent.2. The composition of wherein the sulfonate composition is one or more members selected from the group consisting of alkanesulfonates claim 1 , alkenesulfonates claim 1 , hydroxyalkanesulfonates claim 1 , and sultones.3. The composition of wherein the acid or ester derivative has at least 1 mole % of trans-Δunsaturation.4. The composition of wherein the sulfonating agent is selected from the group consisting of sulfur trioxide claim 1 , sulfuric acid claim 1 , fuming sulfuric acid claim 1 , and chlorosulfonic acid.5. The composition of wherein the sulfitating agent is selected from the group consisting of alkali metal sulfites and bisulfites.6. The composition of wherein the reaction product comprises a sultone.7. The composition of wherein the sultone is a β- claim 6 , γ- claim 6 , or δ-sultone.8. The composition of wherein the reaction product comprises an alkanesulfonate.11. The composition of wherein the ...

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Номер записи: 31
29-08-2013 дата публикации

PROCESS FOR THE PREPARATION OF TRYPTASE INHIBITORS

Номер: US20130225825A1
Автор: GRAF Claus-Dieter, SLEDESKI Adam W., TAPPERTZHOFEN Christoph
Принадлежит: SANOFI-AVENTIS DEUTSCHLAND GMBH

This invention is directed to processes for the preparation of a compound of the formula I or salt thereof, 2. A process according to for the preparation of 4-[3-(tert-butoxycarbonylaminomethyl)phenyl]piperidine or its salt claim 1 ,comprisinga) treating 3-bromobenzylamine hydrochloride or 3-iodobenzylamine hydrochloride with 1,2-bis(chlorodimethylsilyl)ethane in a halogenated aliphatic hydrocarbon in the presence of a tertiary amine to provide the corresponding 1-(3-halobenzyl)-2,2,5,5-tetramethyl-1-aza-2,5-disilacyclopentane, where halo is bromo or iodo;b) treating the 1-(3-halobenzyl)-2,2,5,5-tetramethyl-1-aza-2,5-disilacyclopentane in an ether with an alkyllithium compound and 1-benzyl-4-piperidone at a temperature of from about −80° C. to about −40° C. to provide 1-[3-(1-benzyl-4-hydroxypiperidin-4-yl)benzyl]-2,2,5,5-tetramethyl-1-aza-2,5-disilacyclopentane;c) treating the 1-[3-(1-benzyl-4-hydroxypiperidin-4-yl)benzyl]-2,2,5,5-tetramethyl-1-aza-2,5-disilacyclopentane with an inorganic acid in a halogenated hydrocarbon to provide 3-(1-benzyl-4-hydroxypiperidin-4-yl)benzylamine as the salt of the inorganic acid;d) treating the 3-(1-benzyl-4-hydroxypiperidin-4-yl)benzylamine with a concentrated, non-oxidizing acid at a temperature of from about 70° C. to about 150° C., followed by alkalinization to provide 3-(1-benzyl-1,2,3,6-tetrahydropyridin-4-yl)benzylamine; ande) treating the 3-(1-benzyl-1,2,3,6-tetrahydropyridin-4-yl)benzylamine with di-tert-butyl dicarbonate in an aliphatic alcohol, ethyl acetate, an ether, a halogenated hydrocarbon, a mixture of two or more of such solvents or a mixture of one or more of such solvents with water, in the presence of an alkali metal hydroxide, carbonate or alcoholate or a tertiary amine to provide 3-(1-benzyl-1,2,3,6-tetrahydropyridin-4-yl)benzylcarbamic acid tert-butyl ester.3. A process according to claim 1 , further comprising treating the amine of the formula XII with hydrogen in a solvent in the presence of a palladium ...

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Номер записи: 32
05-09-2013 дата публикации

CRYSTAL OF 6,7-UNSATURATED-7-CARBAMOYL MORPHINAN DERIVATIVE AND METHOD FOR PRODUCING THE SAME

Номер: US20130231485A1
Автор: Haga Nobuhiro, Inagaki Masanao, Morimoto Kenji, Noguchi Kouichi, Oda Shinichi, Omura Sohei, Tamura Yoshinori
Принадлежит:

Stable crystalline forms of a compound represented by the formula (IA): 3. The crystal of the p-toluenesulfonic acid salt according to claim 2 , wherein the crystal has peaks in diffraction angles (2θ) of: 7.8°±0.2° claim 2 , 10.6°±0.2° claim 2 , 15.6°±0.2° claim 2 , 17.8°±0.2° and 21.5°±0.2° in an X-ray powder diffraction spectrum.4. The crystal of the p-toluenesulfonic acid salt according to claim 2 , wherein the crystal has peaks in diffraction angles (2θ) of: 7.8°±0.2° claim 2 , 10.6°±0.2° claim 2 , 15.6°±0.2° claim 2 , 17.8°±0.2° claim 2 , 18.6°±0.2° claim 2 , 20.4°±0.2° claim 2 , 21.5°±0.2° claim 2 , 21.9°±0.2° claim 2 , 23.6°±0.2° and 25.5°±0.2° in an X-ray powder diffraction spectrum.5. The crystal of the p-toluenesulfonic acid salt according to claim 2 , wherein an X-ray powder diffraction spectrum of the crystal is substantially identical with .6. A form I crystal of the p-toluenesulfonic acid salt hydrate according to claim 2 , wherein the crystal has peaks in diffraction angles (2θ) of: 12.9°±0.2° claim 2 , 17.6°±0.2° claim 2 , 22.4°±0.2° claim 2 , 25.4°±0.2° and 28.7°±0.2° in an X-ray powder diffraction spectrum.7. The form I crystal of the p-toluenesulfonic acid salt hydrate according to claim 2 , wherein the crystal has peaks in diffraction angles (2θ) of: 6.6°±0.2° claim 2 , 8.9°±0.2° claim 2 , 11.4°±0.2° claim 2 , 12.9°±0.2° claim 2 , 14.0°±0.2° claim 2 , 15.0°±0.2° claim 2 , 17.6°±0.2° claim 2 , 18.2°±0.2° claim 2 , 22.4°±0.2° claim 2 , 25.4°±0.2° and 28.7°±0.2° in an X-ray powder diffraction spectrum.8. The form I crystal of the p-toluenesulfonic acid salt hydrate according to claim 2 , wherein an X-ray powder diffraction spectrum of the crystal is substantially identical with .9. A form II crystal of the p-toluenesulfonic acid salt hydrate according to claim 2 , wherein the crystal has peaks in diffraction angles (2θ) of: 8.8°±0.2° claim 2 , 17.5°±0.2° claim 2 , 21.9°±0.2° claim 2 , 23.7°±0.2° and 26.1°±0.2° in an X-ray powder diffraction ...

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Номер записи: 33
19-09-2013 дата публикации

SULFONATION IN CONTINUOUS-FLOW MICROREACTORS

Номер: US20130245315A1
Автор: Winter Marc, Zhang Feixia
Принадлежит:

A continuous flow process for sulfonating 1,2.diaminobenzene comprises introducing a sulfonation mixture into a microreactor inlet of a continuous flow microreactor to produce a flow of the sulfonation mixture through the continuous flow microreactor. The sulfonation mixture comprises 1,2 aminobenzene dissolved in a molar excess of sulfuric acid. The continuous flow microreactor comprises one or more individual fluidic modules each having various features with respect to channel width and thermal management. The process further comprises maintaining a reaction temperature of from about 150.230 deg C. in at least a portion of the individual fluidic modules while the sulfonation mixture flows from the microreactor inlet to the microreactor outlet. Thereupon, the sulfonation mixture is received from the microreactor outlet. Finally, a sulfonated reaction product is precipitated out of the sulfonation mixture received from the microreactor outlet. The sulfonated reaction product is 3,4.diaminosulfonic acid, free of doubly sulfonated impurities. 1. A continuous-flow process for sulfonating 1 ,2-diaminobenzene , the continuous-flow process comprising: each individual fluidic module comprises a module inlet and a module outlet, the module inlet in fluidic communication with the module outlet;', 'each individual fluidic module comprises a continuous channel defined in a reaction volume of the individual fluidic module, the continuous channel defining a tortuous fluidic flowpath from a reaction-volume inlet of the reaction volume to a reaction-volume outlet of the reaction volume, the reaction-volume inlet being in fluidic communication with the module outlet, the reaction-volume outlet being in fluidic communication with the module outlet, the continuous channel having a continuous-channel width of from 0.4 mm to 6 mm;', 'one individual fluidic module is an inlet module, such that an inlet-module inlet of the inlet module defines the microreactor inlet;', 'one individual ...

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Номер записи: 34
03-10-2013 дата публикации

PHENOXYPROPANOL DERIVATIVES AND THEIR USE IN TREATING CARDIAC AND CARDIOVASCULAR DISEASES

Номер: US20130261178A1
Автор: Baker Jillian Glenda, Daras Etienne, Fischer Peter Martin, Fromont Christophe, Hill Stephen John, Jadhav Gopal, Kellam Barrie, Mistry Shailesh
Принадлежит:

A compound of formula I-0, and its pharmaceutically acceptable salt or salts and physiologically hydrolysable derivatives in free form or salt form: 2. The compound as claimed in wherein Ris selected from unsubstituted and substituted Ccycloalkyl claim 1 , Ccycloalkyl-Calkyl claim 1 , Calkyl claim 1 , Caryl-Calkyl claim 1 , Calkoxy-Caryl-Calkyl.3. The compound as claimed in wherein Xis selected from CO claim 1 , CS claim 1 , SOand a single bond.4. The compound as claimed in wherein Rand Rare selected from ROZO as hereinbefore defined claim 1 , m- claim 1 ,p-(OCH)or o- claim 1 , m- or p-OH claim 1 , F claim 1 , Cl claim 1 , Br claim 1 , NH claim 1 , R claim 1 , OR claim 1 , or CFor a combination thereof.12. A process for the preparation of a compound of formula I-0 or subformulae as defined in .14. A composition comprising a therapeutically effective amount of a compound of formula I-0 or subformulae or its pharmaceutically acceptable salt and physiologically hydrolysable derivative as defined in in association with one or more pharmaceutical carriers or diluents.15. The use of a compound of formula I-0 or subformulae or pharmaceutically acceptable salt or composition as defined in in the prevention or treatment of a condition selected from ischaemic heart disease claim 1 , hypertension and heart failure claim 1 , more preferably with concomitant respiratory disease claim 1 , in particular asthma or COPD.16. A method of treating a condition selected from ischaemic heart disease (also known as myocardial infarction or angina) claim 1 , hypertension and heart failure claim 1 , restenosis and cardiomyopathy claim 1 , more preferably with concomitant respiratory disease claim 1 , in particular asthma or COPD claim 1 , said method comprising administering to a subject in need thereof claim 1 , a compound of formula I-0 or subformulae or pharmaceutically acceptable salt or composition thereof as defined in in an amount sufficient to treat the condition.17. A method of ...

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Номер записи: 35
03-10-2013 дата публикации

Polymorphic Form of N-(S)-(3,4-Difluoro-2-(2-Fluoro-4-Iodophenylamino)-6-Methoxyphenyl)-1-(2,3-Dihydroxypropyl)Cyclopropane-1-Sulfonamide and uses thereof

Номер: US20130261339A1
Автор: Stuart Dimock
Принадлежит: Ardea Biociences Inc

Disclosed herein, in certain embodiments, is a crystalline polymorph form A of N—(S)-(3,4-difluoro-2-(2-fluoro-4-iodophenylamino)-6-methoxyphenyl)-1-(2,3-dihydroxypropyl)cyclopropane-1-sulfonamide. Further disclosed herein, in certain embodiments, are pharmaceutical compositions comprising the crystalline polymorph form A of N—(S)-(3,4-difluoro-2-(2-fluoro-4-iodophenylamino)-6-methoxyphenyl)-1-(2,3-dihydroxypropyl)cyclopropane-1-sulfonamide.

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Номер записи: 36
10-10-2013 дата публикации

Purificiation of precursor compound by crystallisation

Номер: US20130267730A1
Автор: Anne Nilsen, Sondre NILSEN
Принадлежит: GE Healthcare Ltd

The invention relates to a process for preparation of radiopharmaceutical precursors, and in particular protected amino acid derivatives which are used as precursors for production of radiolabelled amino acids for use in vivo imaging procedures such as positron emission tomography (PET). Particularly, the invention relates to a process for preparation of a precursor useful in the preparation of the [ 18 F]-1-amino-3-fluorocyclobutanecarboxylic acid ([ 18 F] FACBC) PET tracer.

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Номер записи: 37
31-10-2013 дата публикации

Novel process for the preparation of bazedoxifene acetate and intermediates thereof

Номер: US20130289296A1
Автор: Bolneni Nageswara Rao, Dandu Venkata Suresh, Gundu Rao Padakandla, Murali Krishna Prasad Divi
Принадлежит: Divis Laboratories Ltd

A novel process is described for the preparation of pharmaceutically useful compounds such as 1-{4-[2-(azepan-1-yl)ethoxy]benzyl}-2-(4-hydroxyphenyl)-3-methyl-1H-indol-5-ol acetic acid commonly known as bazedoxifene acetate of the formula-1 using 2-(4-{[5-(benzyloxy)-2-[4-(benzyloxy)phenyl]-3-methyl-1H-indol-1-yl]methyl}phenoxy)ethyl-4-methylbenzenzene-1-sulfonate (formula 2a)

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Номер записи: 38
21-11-2013 дата публикации

PROCESS FOR PREPARATION OF ISOSULFAN BLUE

Номер: US20130310600A1
Автор: Kovi Ravishanker, Nampalli Satyam, Tharial Peter Xavier
Принадлежит: APICORE, LLC

A process for the preparation of isosulfan blue (Active Pharmaceutical Ingredient) is provided. A process is also provided for preparation of the intermediate, 2-chlorobenzaldehyde-5-sulfonic acid, sodium salt of formula (2), used in the preparation thereof and a procedure for the isolation of benzaldehyde-2,5-disulfonic acid, di-sodium salt of the formula (3). Also provided is a process for the preparation of an isoleuco acid of formula (4), which upon mild oxidation gives rise to isosulfan blue of pharmaceutical grade which can be used for preparation of pharmaceutical formulations. The isolation and purification procedures provided in the process provide substantially pure isosulfan blue with HPLC purity 99.5% or greater. 3. The process of preparing 2-chlorobenzaldehyde-5-sulfonic acid claim 2 , sodium salt of formula (2) according to comprising reacting 2-chlorobenzaldehyde with sulfuric acid.4. The process according to wherein the polar solvent is methanol.6. The process according to wherein the reaction is carried out in a pressure vessel at 170-180° C. for 5 to 7 hours.7. The process according to wherein the reaction is carried out under a pressure of 140 to 150 psi.8. The process according to comprising precipitating inorganic salts which will hinder the rate of reaction using methanol or one or more Clower alcohols.9. The process according to in which the benzaldehyde-2 claim 2 ,5-disulfonic acid disodium salt is purified by extracting with a non-aqueous polar solvent followed by its precipitation in a halogenated or non-halogenated non-polar solvent which is miscible with the non-aqueous polar solvent.10. The process according to wherein the nonaqueous polar solvent is N claim 9 ,N dimethylformamide and the nonpolar solvent is dichloromethane.12. The process according to performed at reflux conditions for 20-25 hours at 115 to 120° C.13. The process according to comprising precipitating a crude solid using methanol or a Clower alcohol.14. The process ...

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Номер записи: 39
12-12-2013 дата публикации

Halogenated Pyrazolo[1,5-A]Pyrimidines, Processes, Uses, Compositions and Intermediates

Номер: US20130331610A1
Автор: Anglada Luis, Guglietta Antonio, Palomer Albert
Принадлежит: Ferrer Internacional, S.A.

The invention provides novel halogenated pyrazolo[1,5-a]pyrimidines of formula (I) wherein R, R, X and Y have different meanings, and pharmaceutically acceptable salts thereof. Compounds of formula (I) are useful for treating or preventing anxiety, epilepsy and sleep disorders including insomnia, and for inducing sedation-hypnosis, anesthesia, sleep and muscle relaxation. The invention also provides synthetic procedures for preparing said compounds and certain intermediates, as well as intermediates themselves. 2. The process of wherein the hydride compound is sodium hydride and Z is iodine.6. An intermediate enaminone compound which is selected from the group consisting of:N-[5-(3-dimethylamino-acryloyl)-2-fluoro-phenyl]-N-methyl-acetamide;N-[2-chloro-5-(3-dimethylamino-acryloyl)-phenyl]-N-methyl-acetamide;N-[5-(3-dimethylamino-acryloyl)-2-fluoro-phenyl]-N-methyl-methanesulfonamide;N-[2-chloro-5-(3-dimethylamino-acryloyl)-phenyl]-N-methyl-methanesulfonamide; andN-[5-(3-dimethylamino-acryloyl)-2-fluoro-phenyl]-N-prop-2-ynyl-methanesulfonamide. This application is a Divisional Application of U.S. patent application Ser. No. 11/922,602, filed Apr. 30, 2009, which is the U.S. National Phase of PCT/EP2006/063243, filed Jun. 15, 2006, which claims benefit of Provisional Application No. 60/692,866 filed on Jun. 21, 2005. This application also claims priority under 35 U.S.C. §119(a) to European Patent Application No. 05105478.1, filed in Europe on Jun. 21, 2005, the entire contents of which are hereby incorporated by reference.This invention is directed to agents with affinity for GABAreceptor, specifically to halogenated pyrazolo[1,5-a]pyrimidines, and more specifically to [7-(3-amino-4-halophenyl)-pyrazolo[1,5-a]pyrimidin-3-yl]-thiophen-2-yl-methanone acyl and sulfonyl compounds.GABAreceptor (γ-aminobutyric acid) is a pentameric protein which forms a membrane ion channel. GABAreceptor is implicated in the regulation of sedation, anxiety, muscle tone, epileptogenic ...

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Номер записи: 40
26-12-2013 дата публикации

method for preparing 2-(N-substituted)-amino-benzimidazole derivatives

Номер: US20130345436A1
Автор: Limin Que, Tong Cai, Yueheng Jiang, Zhigang Lin
Принадлежит: ABA Chemicals Corp

A method for preparing 2-(N-substituted)-amino-benzimidazole derivatives is provided, which comprises the following steps: (1) reacting a compound of 2-(N-protecting group)-O-aryl diamine with a compound of N-phenoxycarbonyl monosubstituted amine to obtain a compound of 2-(N-protecting group)-amino aryl urea; (2) in a suitable organic solvent, performing dehydrating cyclization reaction of the compound of 2-(N-protecting group)-amino aryl urea in the presence of an organic base and dichloro triphenylphosphine prepared by triphenylphosphine oxide with oxalyl chloride or diphosgene or triphosgene, or dibromo triphenylphosphine prepared by triphenylphosphine oxide with bromine, to produce a compound of 1-protecting group-2-(N-substituted)-amino-benzimidazole; (3) deprotecting the resulting compound of 1-protecting group-2-(N-substituted)-amino-benzimidazole to obtain the compound 2-(N-substituted)-amino-benzimidazole.

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Номер записи: 41
02-01-2014 дата публикации

Substituted diphenyl derivatives

Номер: US20140005149A1
Автор: Förster Heinz
Принадлежит:

Triazene-substituted diphenyl derivatives are suitable as chemotherapeutic agents for treating carcinomas in humans and animals. 112-. (canceled)13. A diphenyl derivative containing(i) at least a dialkyltriazenyl group,(ii) at least one sulfooxy group and/or at least one sulfamoyloxy group per molecule, andits salts, solvates and solvates of these salts.21. A method of combating tumors of the skin and of the target organs dependent on sex hormones in human beings and animals by administration of a sufficient amount of at least one diphenyl derivative containing (i) at least one dialkyltriazenyl group , (ii) at least one sulfooxy group and/or at least one sulfamoyloxy group per molecule and its salts , solvates and solvates of these salts.22. A medicament containing at least one of the diphenyl derivatives containing (i) at least one dialkyltriazenyl group , (ii) at least one sulfooxy group and/or at least one sulfamoyloxy group per molecule and their salts , solvates and solvates of these salts , optionally together with one or more pharmacologically acceptable auxiliaries or supports. This application is a National Stage filing of International Application PCT/DE2012/000258, filed Mar. 12, 2012, claiming priority to German Applications No. DE 10 2011 014 087.5 filed Mar. 16, 2011, entitled “Substituted Diphenyl Derivatives.” The subject application claims priority to PCT/DE2012/000258, and to German Applications No. DE 10 2011 014 087.5 and incorporates all by reference herein, in their entirety.The present invention relates to substituted diphenyl derivatives containing at least (i) a dialkyltriazenyl group, (ii) at least one sulfooxy group and/or at least one sulfamoyloxy group per molecule, their salts, solvates and the solvates of these salts. The invention further relates to a process for preparing these compounds and to their use as medicaments.For the purposes of the present invention, diphenyl derivatives are phenyl rings joined by a single bond or by a ...

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Номер записи: 42
02-01-2014 дата публикации

Salts and Polymorphs of a Tetracycline Compound

Номер: US20140005420A1
Автор: Cvetovich Raymond, Warchol Tadeusz
Принадлежит: PARATEK PHARMACEUTICALS, INC.

Crystalline forms, including salts and polymorphs, of a compound useful in the treatment of tetracycline compound-responsive states are provided herein. The crystalline compounds are useful for the treatment or prevention of conditions and disorders such as bacterial infections and neoplasms, as well as other known applications for tetracycline compounds in general. 2. The method of claim 1 , wherein the first solvent or combination of solvents and the second solvent or combination of solvents are the same.3. The method of claim 1 , wherein the first solvent or combination of solvents and the second solvent or combination of solvents are different.4. The method of claim 1 , wherein the first combination of solvents and the second combination of solvents are each independently a combination of alcoholic solvents.5. The method of claim 4 , wherein the first combination of solvents and the second combination of solvents are each independently a combination of two alcoholic solvents.6. The method of claim 5 , wherein the two alcoholic solvents are ethanol and isopropanol.7. The method of claim 6 , wherein the ethanol and isopropanol are at a volume-to-volume ratio of 2 to 1.8. The method of claim 1 , wherein the first combination of solvents and the second combination of solvents each comprises an alcoholic solvent and an anti-solvent.9. The method of claim 8 , wherein the alcoholic solvent is methanol.10. The method of claim 8 , wherein the anti-solvent is selected from a ketone claim 8 , an ester and an ether.11. The method of claim 10 , wherein the ether is methyl-t-butyl ether.12. The method of claim 1 , wherein the first combination of solvents and the second combination of solvents each comprises methanol and methyl-t-butyl ether.13. The method of claim 12 , wherein the methanol and methyl-t-butyl ether are at a volume-to-volume ratio of 1 to 1.2.14. The method of claim 1 , wherein the p-toluenesulfonic acid is provided in an amount of from 25 to 75 wt % relative ...

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Номер записи: 43
09-01-2014 дата публикации

Method for the synthesis of dha

Номер: US20140012024A1
Автор: Mohamed Amin Khan, Paul L. Wood
Принадлежит: Phenomenome Discoveries Inc

A method for preparing docosahexaenoic acid (DHA). The method comprises coupling a compound represented by Formula I with a compound represented by Formula II followed by partial hydrogenation to obtain a compound represented by Formula III. The compound represented by Formula III acts as a DHA precursor and thus can be hydrolysed to obtain DHA. Novel starting materials represented by Formula I and Formula II, and synthetic routes for preparing the same are also provided.

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Номер записи: 44
06-02-2014 дата публикации

Compositions and processes of preparing and using the same

Номер: US20140039182A1
Автор: Changho HAN, David A. Colby, Mark V. RIOFSKI
Принадлежит: PURDUE RESEARCH FOUNDATION

The present invention relates to compositions, for example, the DBU/Hexafluoroacetone hydrate salt, and processes of preparing and using the same for the modification of chemical compounds via the release of trifluoroacetate. The DBU/Hexafluoroacetone hydrate salt can perform trifluoromethylation reactions on chemical compounds, such as carbonyl group-containing compounds.

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Номер записи: 45
06-02-2014 дата публикации

METHOD FOR PRODUCING DIAMINE COMPOUND

Номер: US20140039220A1
Автор: HAKAMATA Tomohiko, Nara Hideki, TOUGE Taichiro
Принадлежит: TAKASAGO INTERNATIONAL CORPORATION

The present invention provides a method for producing a compound represented by general formula (1) (wherein R, R, R, R-R, A-A, nand nare as defined in the description), which is characterized by reacting a compound represented by general formula (2) (wherein R-R, A-A, n, nand B are as defined in the description) with a diamine compound represented by general formula (3) (wherein R-Rare as defined in the description). The present invention is a method for producing a diamine compound, which is useful for the formation of a ruthenium-diamine complex, under mild conditions, said method being able to be put in industrial practice. 2. The production method according to claim 1 , whereinthe reaction of the compound represented by the general formula (2) is reacted with the diamine compound represented by the general formula (3) at a temperature of 100° C. to 200° C. This application is a National Stage of International Application No. PCT/JP2012/061445 filed Apr. 27, 2012, claiming priority based on Japanese Patent Application No. 2011-101528 filed Apr. 28, 2011, the contents of all of which are incorporated herein by reference in their entirety.The present invention relates to a method for producing a diamine compound useful for forming a ruthenium-diamine complex important as an asymmetric reduction catalyst.Many asymmetric reactions including asymmetric reduction have been developed, and many asymmetric reactions have been reported in which asymmetric metal complexes having optically active phosphine ligands are used. On the other hand, many reports have shown that complexes in which optically active nitrogen compounds are coordinated to transition metals, such as ruthenium, rhodium, and iridium, for example, have excellent performances as catalysts for asymmetric synthesis reactions. Moreover, to enhance the performances of these catalysts, various optically active nitrogen compounds have been developed (Non Patent Literatures 1, 2, 3, 4, etc.). In particular, M. ...

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Номер записи: 46
20-02-2014 дата публикации

Patterning process and resist composition

Номер: US20140051026A1
Автор: Jun Hatakeyama, Koji Hasegawa, Masayoshi Sagehashi, Teppei Adachi
Принадлежит: Shin Etsu Chemical Co Ltd

A negative pattern is formed by coating a resist composition comprising a polymer comprising recurring units having a tertiary ester type acid labile group having a plurality of methyl or ethyl groups on alicycle and an acid generator onto a substrate, prebaking, exposing to high-energy radiation, baking, and developing in an organic solvent developer so that the unexposed region of resist film is dissolved away and the exposed region of resist film is not dissolved. The resist composition exhibits a high dissolution contrast during organic solvent development and forms a fine hole or trench pattern of dimensional uniformity.

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Номер записи: 47
27-02-2014 дата публикации

NOVEL COMPOUNDS DERIVED FROM TAURINE, PROCESS OF THEIR PREPARATION AND PHARMACEUTICAL COMPOSITIONS CONTAINING THESE

Номер: US20140057959A1
Автор: Blau Lorena, Chin Chung Man, Longo Maria do Carmo, Menegon Renato Farina, Santos Jean Leandro Dos, Vizioli Ednir de Oliveira
Принадлежит:

The present invention relates to compounds derived from taurine with non-steroidal anti inflammatory activity. 116-. (canceled)18. The process according to claim 17 , wherein the process is a process of latentiation.19. The process according to claim 17 , wherein the NSAI compound is selected from the group consisting of: salycilates claim 17 , pyrazolons and its analogs claim 17 , derived indoleacetics claim 17 , derived arilacetics claim 17 , derived arylpropionics claim 17 , oxycams claim 17 , and phenamates.20. The process according to claim 19 , wherein the NSAI compound is selected from the group consisting of:2-[2-(2,6-dichlorophenylamino)phenyl]acetic acid,2-[(2,6-dichloro-3-methylphenyl)amino]benzoic acid,2-{[3-(trifluoromethyl)phenyl]amino}nicotinic acid,2-[(2,3-dimethylphenyl)amino]benzoic acid,[2-(2,4-dichlorophenoxy)phenyl]acetic acid,2-[(3-chloro-2-methylphenyl)amino]benzoic acid,2-[(1,2-diphenyl-hydrazine) carbonyl]hexanoic acid,4-[(4-butyl-3,5-dioxo-1,2-diphenylpyrazolidin-4-yl)methoxy]-4-oxobutanoic acid,(1,3,4-triphenyl-1H-pyrazol-5-yl)acetic acid,[3-(4-chlorophenyl)-1-phenyl-1H-pyrazol-4-yl]acetic acid,[(1-benzyl-1H-indazole-3-yl)oxy]acetic acid,[4-(4-chlorophenyl)-2-phenyl-1,3-thiazol-5-yl]acetic acid,[2-(4-chlorophenyl)-1,3-thyazol-4-yl]acetic acid,3-(4,5-diphenyl-1,3-oxazol-2-yl)propanoic acid,[1-(4-chlorophenyl)-2,5-dimethyl-1H-pyrol-3-yl]acetic acid,2-amino-6-benzyl-4,5,6,7-tetrahydrothyen[2,3-c]pyridine-3-carboxylic acid,2-(2-hydroxybenzoic)acid,[2-(aminocarbonyl)phenoxy]acetic acid,2,5-dihydroxybenzoic acid,2-(acetyloxy)benzoic acid,2-(sulphooxy)benzoic acid,2-[(2-hydroxybenzoyl)oxy]benzoic acid,2-[(2-phenylethyl)amino]benzoic acid,5-[(2-phenyl-4,5-dihydro-3H-benzo[e]-1H-indole-2-(2-hydroxybenzoic acid),2′,4′-difluoro-4-hydroxy-1,1′-diphenyl-3-carboxilic acid,2-(4-isobutylphenyl) butanoic acid,2-(4-isobutylphenyl) propanoic acid,2-[4-(thyen-2-yl-carbonyl)phenyl]propanoic acid,2-(3-phenoxyphenyl) propanoic acid,chloro(3-chloro-4-cyclo- ...

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Номер записи: 48
06-03-2014 дата публикации

Composition and Methods for Modulating a Kinase Cascade

Номер: US20140066445A1
Автор: Hangauer, JR. David G.
Принадлежит:

The invention relates to compounds and methods for modulating one or more components of a kinase cascade. The invention also relates to substantially pure compound 1 and substantially pure compound 1 salt (e.g., compound 1 hydrochloride salt and compound 1 benzenesulfonate salt). The invention further relates to methods of preparing substantially pure compound 1 and compound 1 salts. 2. The composition of claim 1 , further comprising a pharmaceutically acceptable carrier or excipient.3. A composition comprising a compound 1 salt having a purity greater than 98.0% as determined by HPLC.4. The composition of claim 3 , wherein the salt is benzenesulfonate salt.5. The composition of claim 3 , further comprising a pharmaceutically acceptable carrier or excipient.6. A method of modulating one or more components of a protein kinase signaling cascade in a subject claim 1 , comprising administering to the subject the composition of .7. The method of claim 6 , wherein the one or more components of the protein kinase signaling cascade are responsible for the manifestation of a disease or disorder selected from hyperproliferative disorders claim 6 , cancers claim 6 , pre-cancers claim 6 , osteoporosis claim 6 , cardiovascular disorders claim 6 , immune system dysfunction claim 6 , type II diabetes claim 6 , obesity claim 6 , hearing loss claim 6 , and transplant rejection.8. A method of modulating one or more components of a protein kinase signaling cascade claim 2 , in a subject claim 2 , comprising administering to the subject the composition of .9. The method of claim 8 , wherein the one or more components of the protein kinase signaling cascade are responsible for the manifestation of a disease or disorder selected from hyperproliferative disorders claim 8 , cancers claim 8 , pre-cancers claim 8 , osteoporosis claim 8 , cardiovascular disorders claim 8 , immune system dysfunction claim 8 , type II diabetes claim 8 , obesity claim 8 , hearing loss claim 8 , and transplant ...

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Номер записи: 49
20-03-2014 дата публикации

Method For The Preparation of Low Overbased Alkyltoluene Sulfonate

Номер: US20140081043A1
Автор: Campbell Curt B., Frederic Kyle J., Gandon Christine Boemare, Sinquin Gilles P., Spala Eugene E., Tequi Pierre
Принадлежит:

Disclosed is a method for improving filtration in the preparation of an alkaline earth metal alkyltoluene sulfonate concentrate by selectively controlling the meta, ortho, para isomer distribution of the alkyl group of the alkyltoluene produced by the process comprising alkylating toluene with at least one isomerized normal alpha olefin, having from about 18 to about 30 carbon atoms and having from 20% to 100% branching in an alkylation process which includes monitoring % isomer formation and adjusting an alkylation process parameter in order to provide a target specified isomer content of less than 38% meta-isomer content; and thereafter sulfonating and neutralizing to produce a low base number sulfonated alkyltoluene concentrate having a Base Number of about 2 to 60 (ASTM D 2896). 1. A method for improving filterability in the preparation of an alkaline earth metal alkyltoluene sulfonate concentrate which comprises:(a) monitoring the isomeric distribution of at least one alkyltoluene produced by alkylating toluene with an olefin comprising at least one isomerized normal alpha olefin, said isomerized normal alpha olefin having from about 18 to about 30 carbon atoms and having from 15% to 100% branching;(b) adjusting at least one alkylation process parameter in order to provide a target isomer distribution having a 2-tolyl C24 isomer content of less than 38% meta, relative to the total 2-tolyl C24 isomer content;(c) sulfonating the alkyltoluene to produce an alkyltoluene sulfonic acid;(d) neutralizing the alkyltoluene sulfonic acid with a source of an alkaline earth metal to provide a neutralized alkyltoluene sulfonate concentrate having a base number of from about 2 to about 60.2. The method of wherein in step b) the alkylation process parameter is selected from the group consisting of adjusting the feed temperature of at least one reactant claim 1 , adjusting the charge mole ratio of the reactants claim 1 , and adjusting the weight hourly space velocity of the ...

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Номер записи: 50
10-04-2014 дата публикации

PROCESS FOR REMOVING DIOXANE FROM A COMPOSITION

Номер: US20140100382A1
Автор: Brooks Burton, Jessup Walter A., Sheats W. Brad
Принадлежит: The Chemithon Corporation

Apparatus and processes for removing dioxane from a composition, e.g., an ethoxylated fatty alcohol sulfate paste, utilize an evaporator having an inlet chamber and one or more heated channels. The process includes the step of heating the composition at a location upstream of the flow restriction to a temperature above the flashing temperature of water at a pressure of the channel inlet and applying a pressure to the heated composition to avoid such flashing. The process further includes the step of passing the pressurized, heated composition through the evaporator. The process can further include injecting a vapor into the channel. The purified, concentrated product can be diluted with water to a desired concentration. 2. The process according to claim 1 , further comprising diluting the concentrated product with water.3. The process according to claim 2 , comprising diluting the concentrated product to a concentration of about 65 wt. % to about 76 wt. % active sulfate.4. The process according to claim 2 , further comprising adjusting the pH of the diluted product by addition of a neutralizing agent.5. The process according to claim 1 , wherein the evaporator comprises a wiped film evaporator.6. The process according to claim 1 , wherein the evaporator comprises a channel and further comprising preheating the dioxane-containing paste feedstock to a temperature wherein water would flash from the paste claim 1 , and selectively applying pressure to the paste to avoid vaporization of water; pumping the paste to an inlet of the channel under a pressure selected to avoid flashing of water; introducing the paste into the channel; supplying heat to the paste in the channel and selectively reducing the pressure along the channel resulting in the flashing of dioxane and water components of the paste claim 1 , wherein vapor liberated during the flashing acts as a motive force to move the increasingly viscous paste along the channel; collecting the resulting concentrated ...

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Номер записи: 51
02-01-2020 дата публикации

Radical initiators and chain extenders for converting methane gas into methane-sulfonic acid

Номер: US20200002276A1
Автор: Alan K. Richards
Принадлежит: Individual

Improved initiators, solvents, and SO3 mixtures are disclosed which can increase the yields and efficiency of a process which converts methane gas into methane-sulfonic acid (MSA). MSA is valuable in its own right, or it can be processed to create desulfured fuels and other chemicals. Preferred initiators have been identified, comprising at least one “primary” initiator, and at least one “extender” (or secondary, supplemental, enhancing, tuning, tweaking, or similar terms) initiator. “Primary” initiator(s) include (unmethylated) Marshall's acid, mono-methyl-Marshall's acid, and di-methyl-Marshall's acid, while a secondary/extender initiator comprises methyl-Caro's acid, which can oxidize sulfur DI-oxide (an unwanted chain terminator) into sulfur TRI-oxide (an essential reagent). Other enhancements to the MSA manufacturing process also are described.

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Номер записи: 52
07-01-2021 дата публикации

HEAT SENSITIVE RECORDING MATERIAL AND COLOR DEVELOPER

Номер: US20210002215A1
Автор: "ONeil Robert Montgomery", BACHMANN Frank, Feiler Leonhard, KOLAMBKAR Prachin, Kulkarni Priti, WAKHARE Vilas
Принадлежит: SOLENIS TECHNOLOGIES CAYMAN, L.P.

The presently claimed invention relates to a color developer, a process for its manufacture and its use as a component in heat sensitive recording material. The heat sensitive recording material is useful for thermographic printing. 40. The compound according to claim 3 , wherein the compound is a crystalline polymorph form α that is characterized by an X-ray powder diffraction pattern comprising 2Θ reflections claim 3 , plus or minus 0.2 degrees 2Θ claim 3 , at 5.5 claim 3 , 6.1 claim 3 , 6.4 claim 3 , 12.1 claim 3 , 16.1 claim 3 , 16.8 claim 3 , 17.1 claim 3 , 18.3 claim 3 , 19.1 claim 3 , 19.9 claim 3 , 20.2 claim 3 , 21.4 claim 3 , 22.1 claim 3 , 22.7 claim 3 , 23.3 claim 3 , 24.3 claim 3 , 24.7 claim 3 , 25.0 claim 3 , 26.4 claim 3 , 27.7 and 29.3.5. The compound according to claim 3 , wherein the compound is a crystalline polymorph form β that is characterized by an X-ray powder diffraction pattern comprising 2Θ reflections claim 3 , plus or minus 0.2 degrees 2Θ claim 3 , at 6.2 claim 3 , 8.1 claim 3 , 10.1 claim 3 , 11.8 claim 3 , 12.2 claim 3 ,13.4 claim 3 , 14.1 claim 3 , 15.3 claim 3 , 16.1 claim 3 ,17.2 claim 3 ,18.4 claim 3 , 19.1 claim 3 , 20.6 claim 3 , 21.4 claim 3 , 22.4 claim 3 , 24.5 claim 3 , 25.0 claim 3 , 25.9 claim 3 , 26.2 claim 3 , 26.9 and 28.4.7. The process according to claim 6 , wherein the chlorination agent is selected from the group of thionyl chloride claim 6 , POCl claim 6 , PCland oxalyl chloride.8. The process according to claim 6 , wherein acid chloride (IVb) is 5-sulfonylchloride-isophthalic acid dichloride.10. The process according to claim 6 , wherein step c. comprises reacting the acid chloride of formula (IVb) with an amine RNHto obtain compound of formula (I) claim 6 , wherein Ris identical to R.11. The process according to claim 6 , wherein the amine is m-toluidine.13. (canceled)15. The heat sensitive recording material according to claim 14 , wherein the weight ratio of color developer to color former is in the range of 1. ...

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Номер записи: 53
07-01-2021 дата публикации

PROCESS FOR PRODUCTION OF GLYCOPYRRONIUM TOSYLATE

Номер: US20210002219A1
Автор: Molteni Renato, SHAW Anthony Adrian, Vigano Enrico
Принадлежит:

Provided herein are methods for the production of glycopyrronium tosylate and glycopyrronium tosylate compositions. Also provided herein are compositions useful in the production of glycopyrronium tosylate. Additionally provided herein are glycopyrronium tosylate compositions. Glycopyrronium tosylate is useful for the treatment of, among other conditions, hyperhidrosis. 119-. (canceled)20. A glycopyrrolate base composition comprising threo-glycopyrrolate base and erythro-glycopyrrolate base , wherein the threo-glycopyrrolate base is at least 95% of the total glycopyrrolate base content of the composition and the erythro-glycopyrrolate base is less than 5% of the total glycopyrrolate base content of the composition.21. The glycopyrrolate base composition of claim 20 , wherein the threo-glycopyrrolate base is at least 96% of the total glycopyrrolate base content of the composition and the erythro-glycopyrrolate base is less than 4% of the total glycopyrrolate base content of the composition.22. The glycopyrrolate base composition of claim 20 , wherein the threo-glycopyrrolate base is at least 97% of the total glycopyrrolate base content of the composition and the erythro-glycopyrrolate base is less than 3% of the total glycopyrrolate base content of the composition.24. A glycopyrronium tosylate composition comprising threo-glycopyrronium tosylate and erythro-glycopyrronium tosylate claim 20 , wherein the threo glycopyrronium tosylate is at least 95% of the total glycopyrrolate tosylate content of the composition and the erythro-glycopyrronium tosylate is less than 5% of the total glycopyrronium tosylate content of the composition.25. The glycopyrronium tosylate composition of claim 24 , wherein the threo-glycopyrronium tosylate is at least 96% of the total glycopyrronium tosylate content of the composition and the erythro-glycopyrronium tosylate is less than 4% of the total glycopyrronium tosylate content of the composition.26. The glycopyrronium tosylate composition ...

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Номер записи: 54
01-01-2015 дата публикации

METHODS AND INTERMEDIATES FOR PREPARING PHARMACEUTICAL AGENTS

Номер: US20150005493A1
Автор: Cordeau Doug, Cullen Aaron, Dowdy Eric, Easton-Scott Leah, Kent Kenneth, Pfeiffer Steven, POLNIASZEK Richard, TRAN Duong, Yu Richard, Zhou Zhongxin
Принадлежит:

The invention provides methods and intermediates that are useful for preparing a compound of formula I: 7. The method of wherein each Ris dimethylaminosulfonyl.9. The method of further comprising preparing the compound of formula II by reacting (S)-2-benzylaziridine with a compound R—X claim 8 , wherein X is a leaving group.18. The method of further comprising preparing the compound of formula XI by treating L-methionine with a corresponding alkylating agent in the presence of water and acetic acid and optionally protecting the resulting amine. This application claims priority to U.S. Provisional Patent Application No. 61/166,498 filed 3 Apr. 2009. The entire content of this application is hereby incorporated herein by reference.International Patent Application Publication Number WO 2008/010921 and International Patent Application Publication Number WO 2008/103949 disclose certain compounds that are reported to be useful to modify the pharmacokinetics of a co-administered drug, e.g. by inhibiting cytochrome P450 monooxygenase. One specific compound identified therein is a compound of the following formula I:There is currently a need for improved synthetic methods and intermediates that can be used to prepare the compound of formula I and its salts. There is also a need for improved methods for preparing intermediate compounds that can be used to prepare the compound of formula I and its salts. The improved methods and intermediates may reduce the cost, time, and/or the amount of waste associated with the existing methods for preparing the compound of formula I and its salts.An improved synthetic route for preparing the compound of formula I and its salts has been identified. This improved synthetic route utilizes novel intermediates of formulae IV, V, XIV, XVI, XVII, and XVIII, identified herein below.This route reduces the cost, the time, and the amount of waste associated with the preparation of the compound of formula I and its salts.Accordingly in one embodiment ...

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Номер записи: 55
20-01-2022 дата публикации

COMPOSITIONS, METHODS, AND SYSTEMS FOR THE SYNTHESIS AND USE OF IMAGING AGENTS

Номер: US20220017459A1
Автор: Benites Pedro, Lazewatsky Joel, Lee L. Veronica, Purohit Ajay, Radeke Heike S.
Принадлежит: Lantheus Medical Imaging, Inc.

The present invention generally relates to novel synthetic methods, systems, kits, salts, and precursors useful in medical imaging. In some embodiments, the present invention provides compositions comprising an imaging agent precursor, which may be formed using the synthetic methods described herein. An imaging agent may be converted to an imaging agent using the methods described herein. In some cases, the imaging agent is enriched in F. In some cases, an imaging agent including salt forms (e.g., ascorbate salt) may be used to image an area of interest in a subject, including, but not limited to, the heart, cardiovascular system, cardiac vessels, brain, and other organs. 1102-. (canceled)104. The method of claim 103 , wherein the maximum dose of the compound or pharmaceutically acceptable salt thereof that is administered to the subject is approximately 13 mCi or less claim 103 , is between approximately 10 mCi and approximately 13 mCi claim 103 , or is between approximately 8 mCi and approximately 10 mCi.105. The method of claim 103 , wherein the portion of the subject being imaged is at least a portion of the cardiovascular system claim 103 , or at least a portion of a tumor claim 103 , or is at least a portion of the heart.106. The method of claim 103 , further comprising determining the presence or absence of a cardiovascular disease or condition in the subject.107. The method of claim 103 , further comprising:{'claim-ref': {'@idref': 'CLM-00103', 'claim 103'}, 'administering a second dose of the compound or pharmaceutically acceptable salt thereof to the subject at a time subsequent to the dose of ; and'}acquiring at least one image of the portion of the subject after the administration of the second dose.108. The method of claim 107 , further comprising:comparing the at least one image acquired after the first dose with the at least one image acquired after the second dose; anddetermining the presence or absence of differences between the cardiac sympathetic ...

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Номер записи: 56
14-01-2016 дата публикации

HIGHLY Z-SELECTIVE OLEFIN METATHESIS

Номер: US20160008802A1
Автор: Flook Margaret M., Hoveyda Amir H., King Annie J., Schrock Richard R., Zhao Yu
Принадлежит:

The present invention relates generally to catalysts and processes for the Z-selective formation of internal olefin(s) from terminal olefin(s) via homo-metathesis reactions. 139-. (canceled)41. The metal complex of claim 40 , wherein the ligand containing oxygen bound to M is substituted —O-aryl claim 40 , wherein the aryl group is phenyl.42. The metal complex of claim 40 , the ligand containing oxygen bound to M is substituted —O-aryl claim 40 , wherein the aryl group is biphenyl.43. The metal complex of claim 40 , the ligand containing oxygen bound to M is substituted —O-aryl claim 40 , wherein the aryl group is 1 claim 40 ,2 claim 40 ,3 claim 40 ,4-tetrahydronaphthyl or naphthyl.44. The metal complex of claim 40 , wherein the ligand containing oxygen bound to M is substituted —O-aryl claim 40 , and substituents positioned in close proximity to the metal center are alkylaryl.45. The metal complex of claim 40 , wherein the metal complex is other than W(NAr)(CHCMePh)(Pyr)(HIPTO).46. The metal complex of claim 40 , wherein the ligand containing oxygen bound to M is 3 claim 40 ,3′-di-tert-butyl-5 claim 40 ,5′ claim 40 ,6 claim 40 ,6′-tetramethyl-2′-(trimethylsilyloxy)biphenyl-2-olate (BiphenTMS) claim 40 , 2′-(tert-butyldimethylsilyloxy)-3-mesityl-5 claim 40 ,5′ claim 40 ,6 claim 40 ,6′ claim 40 ,7 claim 40 ,7′ claim 40 ,8 claim 40 ,8′-octahydro-1 claim 40 ,1′-binaphthyl-2-olate (MesBitet) claim 40 , 3 claim 40 ,3′-dimesityl-2′-(tert-butyldimethylsilyloxy)-5 claim 40 ,5′ claim 40 ,6 claim 40 ,6′ claim 40 ,7 claim 40 ,7′ claim 40 ,8 claim 40 ,8′-octahydro-1 claim 40 ,1′-binaphthyl-2-olate (MesBitet) claim 40 , or MesBitetOMe is 3 claim 40 ,3′-dimesityl-2′-methoxy-5 claim 40 ,5′ claim 40 ,6 claim 40 ,6′ claim 40 ,7 claim 40 ,7′ claim 40 ,8 claim 40 ,8′-octahydro-1 claim 40 ,1′-binaphthyl-2-olate (MesBitetOMe).49. The metal complex of claim 48 , wherein Ris tert-butyl claim 48 , optionally substituted.50. The metal complex of claim 48 , wherein Ris substituted phenyl.51. ...

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Номер записи: 57
12-01-2017 дата публикации

LITHIUM STYRENE SULFONATE

Номер: US20170008837A1
Автор: KASAHARA Senshi, SHIRAISHI Chikara
Принадлежит:

To provide a novel lithium styrene sulfonate which is capable of solving a problem of an increase of the production cost due to drying under atmospheric pressure or reduced pressure at a temperature of at least 40° C. and a problem of polymerization of lithium styrene sulfonate. The lithium styrene sulfonate is characterized in that when measured by using a Thermogravimetric-Differential Thermal Analyzer under measuring condition of heating at a temperature raising rate of 2° C./min in a nitrogen stream, the temperature at the top of the main endothermic peak in a range of from 80 to 170° C., is at least 120° C. 110-. (canceled)11. Lithium styrene sulfonate wherein when measured by using a Thermogravimetric-Differential Thermal Analyzer under measuring condition of heating at a temperature raising rate of 2° C./min in a nitrogen stream , the temperature at the top of the main endothermic peak in a range of from 80 to 170° C. , is at least 120° C.12. The lithium styrene sulfonate according to claim 11 , wherein when measured by using a Thermogravimetric-Differential Thermal Analyzer under measuring condition of heating at a temperature raising rate of 2° C./min in a nitrogen stream claim 11 , the weight reduction in a range of from 120 to 170° C. claim 11 , is at least 2.2 wt % claim 11 , and the water content is from 4.0 to 50.0 wt %.13. The lithium styrene sulfonate according to claim 11 , wherein the content of plate crystals is at least 10 area % and at most 100 area %.14. The lithium styrene sulfonate according to claim 11 , wherein the ratio of (long side length/width) of the plate crystals is at most 3.0.15. The lithium styrene sulfonate according to claim 11 , wherein the width of the plate crystals is at least 10 μm.16. The lithium styrene sulfonate according to claim 11 , wherein when measured by a powder X-ray diffraction method by using Cu-Kα radiation claim 11 , at least the intensity of a peak appearing at a diffraction angle of 7.9° is stronger than ...

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Номер записи: 58
14-01-2016 дата публикации

PHOTORESIST MONOMER, PHOTORESIST AND METHOD FOR THE PREPARATION THEREOF, COLOR FILTER

Номер: US20160009641A1
Автор: TANG Chen, Wang Xuelan
Принадлежит: BOE Technology Group Co., Ltd.

A photoresist monomer, a photoresist and a method for the preparation thereof, a color filter. The photoresist monomer has a structure represented by Formula I, 2. The photoresist monomer according to claim 1 , wherein claim 1 , in Formula I claim 1 , m claim 1 , m claim 1 , and mare in the range of 50-400.3. A The photoresist comprising the photoresist monomer of claim 1 , or a mixture of photoresist monomers.4. The photoresist according to claim 3 , wherein claim 3 , said photoresist further comprises an alkaline soluble resin claim 3 , a pigment dispersion claim 3 , a photoinitiator claim 3 , a solvent claim 3 , and an adjuvant; said photoresist comprising claim 3 , in part by weight claim 3 ,photoresist monomer or a mixture of photoresist monomers: 11.2-21.2 parts;alkaline soluble resin: 7.4-19.8 parts;pigment dispersion: 35.2-57.6 parts;photoinitiator: 1.8-11.9 parts;solvent: 11.26-28.5 parts; andadjuvant: 0.07-0.21 part.5. The photoresist according to claim 3 , wherein claim 3 , the mixture of the photoresist monomers comprises photoresist monomers A claim 3 , B claim 3 , and C claim 3 , wherein claim 3 ,the photoresist monomer A has a structure of Formula I in which n is 1, and is in 1 part by weight;the photoresist monomer B has a structure of Formula I in which n is 2, and is in 2.3-4.3 parts by weight; andthe photoresist monomer C has a structure of Formula I in which n is 3, and is in 5.1-5.7 parts by weight.6. The photoresist according to claim 3 , wherein claim 3 , the mixture of the photoresist monomers comprises photoresist monomers A claim 3 , B claim 3 , and D claim 3 , wherein claim 3 ,the photoresist monomer A has a structure of Formula I in which n is 1, and is in 1 part by weight;the photoresist monomer B has a structure of Formula I in which n is 2, and is in 2.7-3.5 parts by weight; andthe photoresist monomer D has a, structure of Formula I in which n is 4, and is in 3.3-5.5 parts by weight.7. The photoresist according to claim 3 , wherein ...

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Номер записи: 59
14-01-2016 дата публикации

CYCLOHEXANEDIAMINE COMPOUNDS AND METHODS FOR THEIR PREPARATION

Номер: US20160009694A1
Автор: Pandey Anjali
Принадлежит:

The present invention provides processes for the preparation of cyclohexanediamine compounds of formula Ia and intermediates thereof. The compounds are useful as Syk kinase inhibitors and in various pharmaceutical compositions, and particularly useful for treating conditions mediated at least in part by Syk kinase activity. 2. The process of claim 1 , wherein step (b) further comprises (i) contacting a compound of Formula (Ic) with a deprotecting reagent and subsequently with a base to provide a compound of Formula (Ia) as a free base; and(ii) optionally contacting the free base of Formula (Ia) with an acid to provide a salt of Formula (Ia).4. The process of claim 1 , wherein X is halo or —S(O)C-Calkyl; and n is 0 claim 1 , 1 or 2.5. The process of claim 1 , wherein P is t-Boc.6. The process of claim 3 , wherein the alkoxide is sodium ethoxide.7. The process of claim 1 , wherein in step (a) X is —SCHwhich is contacted with an oxidizing agent before the compound of Formula (Ib) is contacted with a compound of Formula (II).8. The process of claim 7 , wherein in step (a) the oxidizing agent is 3-chloroperbenzoic acid.9. The process of claim 2 , wherein in step (b) the deprotecting reagent is hydrochloric acid.10. The process of claim 2 , wherein in step (b) the acid is acetic acid and the compound of Formula (Ia) is an acetate salt.12. The process of claim 11 , wherein the compound of Formula (II) has an enantiomeric excess of at least 98% e.e.13. The process of claim 11 , wherein the base is potassium carbonate.16. The process of claim 15 , wherein in step (d) the base is sodium hydroxide.17. The process of claim 15 , wherein in step (e) the reducing agent is Hand Pd(OH).18. The process of claim 15 , wherein in step (f) the alkylsulfonylhalide is methanesulfonyl chloride and Y is —OS(O)CHin Formula (VIII).19. The process of claim 15 , wherein in step (g) a crown ether such as 15-crown-5 is added.20. The process of claim 15 , wherein in step (h) the reducing agent is ...

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Номер записи: 60
14-01-2016 дата публикации

NOVEL PROCESS FOR PREPARING CEFTAROLINE FOSAMIL

Номер: US20160009745A1
Автор: Kremminger Peter, Sturm Hubert
Принадлежит: SANDOZ AG

The present invention relates to a novel process for preparing ceftaroline fosamil via intermediates of Formulae (1), (3) or (4) of this process. 3. The process according to claim 2 , wherein the compound having the formula (11) is an acetate solvate or is transformed into an acetate solvate.5. The process according to claim 4 , wherein Y is selected from the group consisting of halogenides claim 4 , trifluoroacetate claim 4 , methane sulfonate claim 4 , trifluoromethane sulfonate claim 4 , toluene-4-sulfonate claim 4 , tetrafluoroborate claim 4 , acetate claim 4 , hexafluorophosphate and hexafluoroantimonate.6. The process according to claim 4 , wherein Y is selected from the group consisting of halogenides claim 4 , trifluoroacetate claim 4 , methane sulfonate claim 4 , trifluoromethane sulfonate claim 4 , toluene-4-sulfonate claim 4 , tetrafluoroborate claim 4 , acetate claim 4 , hexafluorophosphate and hexafluoroantimonate. This application is a divisional of U.S. application Ser. No. 14/343,723 filed Jun. 12, 2014, entitled NOVEL PROCESS FOR PREPARING CEFTAROLINE FOSAMIL, which is a national stage filing under 35 U.S.C. §371 of International Application No. PCT/EP2012/067550 filed Sep. 7, 2012, which claims priority under 35 U.S.C. §119(b) and 37 CFR 1.55(a) to European Application No. 11180728.5 filed Sep. 9, 2011, the disclosures of all of which are incorporated herein by reference.The present invention relates to a novel process for preparing ceftaroline fosamil as well as to intermediates of this process.Ceftaroline fosamil ((6R,7R)-7-[(2Z)-2-ethoxyimino-2-[5-(phosphonoamino)-1,2,4-thiadiazol-3-yl]acetyl]amino]-3-[4-(1-methylpyridin-1-ium-4-yl)-1,3-thiazol-2-yl]sulfanyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate; Teflaro) is a cephalosporin antibiotic which is active against methicillin-resistant and Gram-positive bacteria. It has the general formulawhereby the compound is generally provided in the form of its acetic acid solvate.EP-A-1 310 ...

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Номер записи: 61
27-01-2022 дата публикации

CLUSTER COMPOUNDS AND METHODS OF MAKING THE SAME

Номер: US20220024865A1
Автор: Bowman Reid Henry, Nicholas David, Singleton Freddie L.
Принадлежит: Earth Science Laboratories, Inc.

Disclosed herein are clusters compounds that include at least one substituted amine sulfate and at least one substituted amine bisulfate molecule. The substituted amine sulfate molecule and the substituted amine bisulfate molecule may each include an ammonium moiety with at least one alkyl substituent. Optionally, the alkyl substituent can include 1 to 20 carbon atoms, 1 to 10 carbon atoms, or 1 to 6 carbon atoms. For example, the alkyl substituent can be a methyl, ethyl, propyl, butyl, or pentyl group. In some examples, the substituted amine sulfate molecule and the substituted amine bisulfate molecule each include an ammonium moiety with at least two alkyl substituents. Optionally, the two alkyl substituents are the same. Alternatively, however, the two alkyl substituents can be different. 1. A cluster compound comprising a cluster of molecules comprising at least one substituted amine sulfate molecule and at least one substituted amine bisulfate molecule.2. The cluster compound of claim 1 , wherein the substituted amine sulfate molecule and the substituted amine bisulfate molecule each comprise an ammonium moiety substituted by at least one alkyl substituent.3. The cluster compound of claim 2 , wherein the at least one alkyl substituent comprises 1 to 20 carbon atoms.4. The cluster compound of claim 3 , wherein the at least one alkyl substituent comprises 1 to 10 carbon atoms.5. The cluster compound of claim 4 , wherein the at least one alkyl substituent comprises 1 to 6 carbon atoms.6. The cluster compound of claim 5 , wherein the at least one alkyl substituent comprises a methyl claim 5 , ethyl claim 5 , propyl claim 5 , butyl claim 5 , or pentyl group.7. The cluster compound of claim 1 , wherein the substituted amine sulfate molecule and the substituted amine bisulfate molecule each comprise an ammonium moiety substituted by at least two alkyl substituents.8. The cluster compound of claim 7 , wherein the at least two alkyl substituents are the same.9. The ...

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Номер записи: 62
11-01-2018 дата публикации

Process for the preparation of a polyunsaturated ketone compound

Номер: US20180009745A1
Автор: Inger-Reidun AUKRUST, Marcel Sanderberg
Принадлежит: Avexxin AS

A process for the preparation of a polyunsaturated thiol comprising: (1) reacting a polyunsaturated alcohol in the presence of a compound of formula R 2 —SO 2 Hal wherein R 2 is a C 1-20 hydrocarbyl group, such an C 1-10 alkyl group, to form a polyunsaturated sulphonyl ester; (2) converting the polyunsaturated sulphonyl ester to a polyunsaturated thioester by reacting with an anion of formula − SC(═O)R 4 wherein R 4 is a C 1-20 hydrocarbyl group; (3) converting the polyunsaturated thioester to form a polyunsaturated thiol optionally in the presence of an antioxidant, e.g. using a metal carbonate. (4) reacting said polyunsaturated thiol with a compound (LG)R 3 COX wherein X is an electron withdrawing group and R 3 is an alkylene group carrying a leaving group (LG), such as LG-CH 2 — forming where X is an electron withdrawing group and LG is a leaving group; optionally in the presence of an antioxidant, so as to form a polyunsaturated ketone compound.

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Номер записи: 63
03-02-2022 дата публикации

CATIONS AS CATALYST IN THE PRODUCTION OF ALKANE SULFONIC ACIDS

Номер: US20220033354A1
Автор: BIERTUEMPEL Ingo, Ott Timo
Принадлежит:

The present invention relates to the use of cations or compounds forming stable cations in the production of alkane sulfonic acids as well as methods to produce methane sulfonic acids employing the cations as catalyst. 1. A process for preparation of alkane sulfonic acids from alkanes and sulfur trioxide , comprising reacting a cation being stable under super acid conditions with alkane to form an alkyl cation , wherein stability means that the cation is able to react with the alkane but does not decompose within 24 h at room temperature (20° C.) , and wherein the cation is a halogen cation.2. The process according to claim 1 , wherein the cation is formed in situ in acid or super acid conditions during the preparation of alkane sulfonic acids.3. The process according to claim 1 , wherein the cation is formed prior to addition to the reaction for obtaining an alkane sulfonic acid.4. The process according to claim 1 , wherein the halogen cation is I+ and Br+ claim 1 , S+ claim 1 , Se+ claim 1 , Te+ claim 1 , As+ claim 1 , Sb+ claim 1 , P+ and/or Si+.5. Process for the preparation of alkane sulfonic acids claim 1 , comprising the steps ofi) providing sulfur trioxide and an alkane to a reaction chamber,ii) setting a pressure of from 1 to 200 bar to the reactor,iii) introducing a compound forming in situ a cation into said reactor, wherein the cation is a halogen cation,iv) controlling the temperature in the reactor to be at 0° C. to 100° C., andv) after the reaction is finished, if necessary, purifying the reaction product.6. Process for the preparation of alkane sulfonic acids claim 1 , comprising the steps ofi) providing sulfur trioxide and an alkane to a reaction chamber,ii) setting a pressure of from 1 to 200 bar to the reactor,iii) introducing a cation being stable under super acid conditions into said reactor, wherein stability means that the cation is able to react with the alkane but does not decompose within 24 h at room temperature (20° C.), and wherein the ...

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Номер записи: 64
03-02-2022 дата публикации

Anionic-cationic-nonionic surfactant, production and use thereof

Номер: US20220033705A1
Автор: Ou SHA, Songyuan GU, Weidong Zhang, Xiaodong Zhai, Xinning BAO, Yingcheng Li, Yiqing YANG, Zhiqin SHEN
Принадлежит: China Petroleum and Chemical Corp, Sinopec Shanghai Research Institute of Petrochemical Technology

An anionic-cationic-nonionic surfactant as substantially represented by the formula (I) exhibits significantly improved interfacial activity and stability as compared with the prior art. With the present anionic-cationic-nonionic surfactant, a flooding fluid composition for tertiary oil recovery with improved oil displacement efficiency and oil washing capability as compared with the prior art could be produced. In the formula (I), each group is as defined in the specification.

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Номер записи: 65
21-01-2016 дата публикации

PREPARATION METHOD OF OPTICALLY ACTIVE DIAMINE COMPOUND

Номер: US20160016974A1
Автор: Kaneda Takeshi, Michida Makoto, NAKAMURA Yoshitaka
Принадлежит: Daiichi Sankyo Company, Limited

The problem to be solved is to provide a method for efficiently producing compounds (1) and (1a) that are important intermediate compounds in the production of FXa inhibitors (X) and (X-a). The solutions thereto are a method for producing a compound represented by the formula (8d) using a stereoselective intramolecular cyclization reaction, and a method for producing a compound (1f) or a salt thereof, or a hydrate thereof, which is characterized by desulfonylation of the compound (8d). In each formula, Rrepresents a C1-C6 alkyl group, a benzyl group, etc. 2. The production method according to claim 1 , wherein the desulfonylation is carried out by treating the compound with water and a base.3. The production method according to claim 2 , wherein the base is a pyridine.6. The production method according to claim 1 , wherein Rand Reach represent an ethyl group.8. The production method according to claim 1 , wherein Rrepresents a C1-C6 alkyl group.9. The production method according to claim 1 , wherein Rrepresents a methyl group.12. The production method according to claim 11 , wherein the desulfonylation is carried out by treating the compound with water and a base.13. The production method according to claim 12 , wherein the base is a pyridine.14. The production method according to claim 1 , wherein Ris a di(methyl)amino group.15. The production method according to claim 1 , wherein Ris a tert-butyl group or a benzyl group.16. The production method according to claim 14 , wherein the compound represented by the formula (1d) or a salt thereof claim 14 , or a hydrate thereof is a sulfate of the compound represented by the formula (1d) claim 14 , an oxalate monohydrate of the compound represented by the formula (1d) claim 14 , or an oxalate of the compound represented by the formula (1d).21. The compound according to claim 20 , wherein Rrepresents a C1-C6 alkyl group.22. The compound according to claim 20 , wherein Rrepresents a methyl group.24. The compound according ...

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Номер записи: 66
18-01-2018 дата публикации

Process for the synthesis of difluoromethyl ether-based compounds

Номер: US20180016227A1
Автор: Abdelmalik Slassi, Peter Dove
Принадлежит: Trillium Therapeutics ULC

The present application relates to a novel process for the preparation of difluoromethyl ether-based derivatives from, for example, aliphatic and aromatic hydroxyl precursors, compositions comprising these compounds and their use, in particular as precursors for medicines for the treatment of diseases, disorders or conditions. In particular, the present application includes the process of preparing compounds of Formula (I), and compositions and uses thereof:

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Номер записи: 67
15-01-2015 дата публикации

Surfactants and Solvents Containing Diels-Alder Adducts

Номер: US20150018563A1
Автор: Bernhardt Randal J., Luxem Franz J., Tabor Rick, Wallace Gregory James, Yao Chunhua
Принадлежит:

Surfactants and solvents containing derivatized adducts formed from Diels-Alder reactions of terpenes and unsaturated carboxylic acids or their derivatives are disclosed. Processes for making and derivatizing the Diels-Alder adducts are also disclosed. 1. A composition comprising a cationic , amine oxide , amphoteric , anionic , or nonionic surfactant which is the reaction product of (a) farnesene or myrcene or mixtures thereof; and', '(b) a dienophile selected from the group consisting of maleic anhydride, itaconic anhydride, dimethyl maleate, dimethyl itaconate, maleic acid, itaconic acid, fumaric acid, dimethyl fumarate, acrylic acid, methyl acrylate, ethyl acrylate, butyl acrylate, methyl methacrylate, methacrylic acid, benzaldehyde, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, acrylonitrile, acrylamide, N-hydroxyethyl maleimide, maleimide, vinyl alkyl ketones, methacrolein, and mixtures thereof; reacted with, '(i) a Diels Alder adduct formed from(ii) at least one derivatizing agent selected from the group consisting of:mono-alkyl ether of polyethylene glycol, mono-alkyl ether of polypropyloxy-polyethyloxy block copolymer, mono-alkyl ethers of polybutyloxy-polyethyloxy block copolymer, amine-containing alkylene glycol, amine-containing polyalkylene glycol, mono- or oligo-alkylene glycol, amine, polyamine, aliphatic alcohol, cycloaliphatic sultone, aromatic substituted alcohol, hydrogenating agent, aryloxy alkylene alcohol, sulfonating agent, phosphating agent, sulfating agent, aryl-alkyl halide, dimethyl sulfate, epichlorohydrin, and combinations thereof.2. The composition of claim 1 , wherein the dienophile is maleic anhydride claim 1 , itaconic anhydride claim 1 , dimethyl maleate claim 1 , dimethyl itaconate claim 1 , maleic acid claim 1 , itaconic acid claim 1 , fumaric acid claim 1 , dimethyl fumarate claim 1 , acrylic acid claim 1 , methyl acrylate claim 1 , ethyl acrylate claim 1 , butyl acrylate ...

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Номер записи: 68
15-01-2015 дата публикации

Processes for isolating fluorinated products

Номер: US20150018587A1
Автор: Junichi Chika, Norimichi Saito, Teruo Umemoto
Принадлежит: UBE Industries Ltd

Useful processes for isolating the fluorinated products formed by reaction with 4-tert-butyl-2,6-dimethylphenylsulfur trifluoride (Fluolead) are disclosed. The processes comprise the conversion of the byproduct (formula I) to sulfinate ester (formula V), and to sulfonate eater (formula VI), and then to the water-soluble sulfonate salt (formula IV) in the presence of the fluorinated products.

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Номер записи: 69
21-01-2021 дата публикации

ORGANIC REACTIONS CARRIED OUT IN AQUEOUS SOLUTION IN THE PRESENCE OF A HYDROXYALKYL(ALKYL)CELLULOSE OR AN ALKYLCELLULOSE

Номер: US20210017100A1
Автор: Braje Wilfried, BRITZE Katarina, Dietrich Justin D., JOLIT Anais, KASCHEL Johannes, KLEE Johanna, Lindner Tanja
Принадлежит:

The present invention relates to a method of carrying out an organic reaction in aqueous solution in the presence of a hydroxyalkyl(alkyl)cellulose or an alkylcellulose. 1. A method of carrying out an organic reaction in a solvent containing at least 90% by weight , based on the total weight of the solvent , of water , which method comprises reacting the reagents in said solvent in the presence of a cellulose derivative as a surfactant which is selected from the group consisting of cellulose modified with one or more alkylene oxides or other hydroxyalkyl precursors , and alkylcellulose;where the organic reaction is not a polymerization or oligomerization reaction of olefinically unsaturated compounds; and [ a transition metal catalyzed C—C coupling reaction:', 'a transition metal catalyzed reaction involving C—N bond formation which is an Au-catalyzed cyclodehydratization of α,β-amino alcohols containing a C—C triple bond:', 'a transition metal catalyzed reaction involving C—O bond formation:', 'a transition metal catalyzed reaction involving C—S bond formation:', 'a transition metal catalyzed reaction involving C—B bond formation: or', 'a transition metal catalyzed reaction involving C-halogen bond formation; or, 'a transition metal catalyzed reaction in which a transition metal catalyst is used; where the transition metal catalyzed reaction is'}, 'a C—C coupling reaction not requiring transition metal catalysis which is selected from the group consisting of reactions of carbonyl or nitrile compounds and pericyclic reactions;, 'where the organic reaction is'}a nucleophilic substitution reaction;a reduction or an oxidation reaction; oran ester formation reaction or an ester hydrolysis reaction.2. The method as claimed in claim 1 , where the cellulose derivative has a viscosity of from 1 to 150000 mPa·s claim 1 , determined as a 2% by weight aqueous solution claim 1 , relative to the weight of water.3. The method as claimed in claim 1 , where in the cellulose ...

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Номер записи: 70
28-01-2016 дата публикации

CRYSTAL OF 6,7-UNSATURATED-7-CARBAMOYL MORPHINAN DERIVATIVE AND METHOD FOR PRODUCING THE SAME

Номер: US20160024102A1
Автор: Haga Nobuhiro, Inagaki Masanao, Morimoto Kenji, Noguchi Kouichi, Oda Shinichi, Omura Sohei, Tamura Yoshinori
Принадлежит: Shionogi & Co., Ltd.

Stable crystalline forms of a compound represented by the formula (IA): 127-. (canceled)3152-. (canceled)53. The process according to to , wherein the salt is a non-solvate.54. The process according to to , wherein the salt is a hydrate. The present invention relates to crystal of a morphinan derivative and a method for producing the same. In more detail, the present invention relates to crystal of a 6,7-unsaturated-7-carbamoyl morphinan derivative, an acid addition salt thereof and/or solvates thereof, and a method for producing the same.In a drug delivery, crystalline forms having useful and outstanding chemical and/or physical properties are desired.The patent document 1 describes that a 6,7-unsaturated-7-carbamoyl morphinan derivative represented by the following formula:is useful as a therapeutic and/or prophylactic agent of the emesis and/or constipation. Although the following compound (1-284):is disclosed in a form of free salt in Examples of the patent, an acid addition salt and/or a solvate are not specifically disclosed. Further, there is no description at all about the crystal thereof. As a method for preparing the 6,7-unsaturated-7-carbamoyl morphinan derivative, all that disclosed is a method for synthesizing a corresponding 7-carbamoyl derivative from 7-carboxy derivative as shown by the following formula:An active ingredient of a medicine may have substantially different physical properties depending on each solid form. Differences in such physical properties may affect a preparation method or administration method of the medicinal active ingredient, or a pharmaceutical composition comprising the active ingredient, for example.Although the 6,7-unsaturated-7-carbamoyl morphinan derivative is already disclosed, establishment of a suitable salt and/or a stable crystal form and a more desirable method for preparing the same has been desired for the drug use or for the industrial drug production.As a result of extensive investigations, inventors of the ...

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Номер записи: 71
17-04-2014 дата публикации

Processes and intermediates for making sweet taste enhancers

Номер: US20140107370A1
Автор: Catherine Tachdjian, Daniel Levin, Donald S. Karanewsky, Peter Leeming, QING Chen, Tayyab Rashid, Xiao-Qing Tang
Принадлежит: Senomyx Inc

The present invention includes methods/processes and intermediates for preparing compounds having structural Formula (I): wherein X is alkyl, substituted alkyl, alkenyl, substituted alkenyl, heteroalkyl, substituted heteroalkyl, heteroalkenyl, or substituted heteroalkenyl.

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Номер записи: 72
25-01-2018 дата публикации

PROCESS FOR FLUORINATION OF SULPHONYL HALIDE COMPOUNDS

Номер: US20180022694A1
Автор: METZ François
Принадлежит:

The present disclosure relates to the preparation of a compound of formula (I) comprising an —SOF function, R—SOF, by reacting a compound of formula (II), R′—SOX, with a fluorinating agent, the process carried out in the liquid phase in the presence of hydrofluoric acid using an antimony-based fluorination catalyst, wherein R, R′, and X are described herein. 1. A non-electrochemical process for preparing a fluorinated compound of formula (I) comprising at least one —SOF function , wherein the compound of formula (I) is prepared by reacting a compound of formula (II) with at least one fluorinating agent , wherein the process is carried out in the liquid phase in the presence of hydrofluoric acid using an antimony-based fluorination catalyst:{'br': None, 'sub': '2', 'R—SOF \u2003\u2003(I)'}where R is selected from the group consisting of R1, R2 and R3:{'sub': n', 'a', 'b, 'R1=—CHFwith n=1-10, a+b=2n+1, b≧1;'}{'sub': x', 'y', 'z', '2, 'R2=—CHF—SOF with x=1-10, y+z=2x and z≧1;'}{'sub': c', 'h', 'f, 'claim-text': {'br': None, 'sub': '2', 'R′—SOX \u2003\u2003(II)'}, 'R3=Φ-CHFwith c=1-10; h+f=2c and f≧1; Φ denoting a phenyl group;'}where R′ is selected from the group consisting of R′1, R′2 and R′3:{'sub': n', 'a', 'b, 'R′1=—CHXwith n=1-10, a+b=2n+1, b≧1;'}{'sub': x', 'y', 'z', '2, 'R′2=—CHX—SOX with x=1-10, y+z=2x and z≧1;'}{'sub': c', 'h', 'f, 'R′3=Φ-CHXwith c=1-10; h+f=2c and f≧1; Φ denoting a phenyl group;'}X is a halogen atom selected from the group consisting of chlorine and bromine.2. The preparation process as claimed in claim 1 , wherein the radicals R1 and R′1 are perhalogenated so that b=3 and a=0.3. The preparation process as claimed in claim 1 , wherein the radical R of the compound (I) is the radical R1 wherein n=1 claim 1 , a=0 and b=3 claim 1 , or n=1 claim 1 , a=1 claim 1 , b=2 or else n=1 claim 1 , a=2 and b=1.4. The preparation process as claimed in claim 1 , wherein the compound of formula (II) is obtained by radical halogenation of a compound of formula ...

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Номер записи: 73
22-01-2015 дата публикации

Methods and Compounds Useful in the Synthesis of Orexin-2 Receptor Antagonists

Номер: US20150025237A1
Автор: Benayoud Farid, Kazuta Yuji, LEE Jaemoon, Moniz George Anthony, Naoe Yoshimitsu, Sorimachi Keiichi, Takemura Ayumi, TANAKA Toshiaki, Terauchi Taro, Wilcoxen Annie Zhu, Yoshida Yu, Zhang Huiming
Принадлежит:

The present disclosure provides compounds and methods that are useful for the preparation of compounds useful as orexin-2 receptor antagonists. 2. The process of claim 1 , wherein Ar is unsubstituted or substituted 1-3 times with a halo independently selected from the group consisting of: chloro claim 1 , fluoro claim 1 , bromo claim 1 , and iodo.3. The process of or claim 1 , wherein said composition is provided at a temperature of from −30 to 30° C.4. The process of or claim 1 , wherein said composition is provided at a temperature of from −30 to 10° C.5. The process of or claim 1 , wherein said composition is provided at a temperature of from −10 to 0° C.6. The process of or claim 1 , wherein said composition is provided at a temperature of from −10 to −5° C.76. The process of any of - claims 1 , wherein the organic solvent is an aromatic hydrocarbon solvent claims 1 , an aliphatic hydrocarbon solvent claims 1 , a halogenated hydrocarbon solvent or an ether solvent.86. The process of any of - claims 1 , wherein the organic solvent is tetrahydrofuran or toluene.96. The process of any of - claims 1 , wherein the organic solvent is a mixture of tetrahydrofuran and 2-methyltetrahydrofuran.109. The process of any of - claims 1 , wherein the hydride reducing agent is selected from the group consisting of: sodium borohydride claims 1 , lithium borohydride claims 1 , lithium aluminum hydride claims 1 , lithium tributoxy aluminum hydride claims 1 , diisobutylaluminum hydride claims 1 , zinc borohydride claims 1 , and lithium triethyl borohydride.119. The process of any of - claims 1 , wherein the hydride reducing agent is lithium borohydride or lithium triethyl borohydride.1211. The process of any of - claims 1 , further comprising the step of mixing the composition after said adding step for a time of 12 to 24 hours.13. The process of claim 11 , further comprising the step of quenching the reduction by adding to said composition a mild aqueous acid.14. The process of ...

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Номер записи: 74
10-02-2022 дата публикации

FLUOROSULFONYL GROUP-CONTAINING COMPOUND, FLUOROSULFONYL GROUP-CONTAINING MONOMER, AND THEIR PRODUCTION METHODS

Номер: US20220041765A1
Автор: Hirai Takeshi, JOMUTA Daisuke, TAMITSUJI Chikaya
Принадлежит: AGC Inc.

A method for producing a fluorosulfonyl group-containing compound to obtain a compound represented by the following formula 5 from a compound represented by the following formula 1 as a starting material and a method for producing a fluorosulfonyl group-containing monomer in which the fluorosulfonyl group-containing compound is used: 2: The fluorosulfonyl group-containing polymer of claim 1 , further comprising copolymerized units of tetrafluoroethylene.3: The fluorosulfonyl group-containing polymer of claim 2 , further comprising a copolymerized unit selected from the group consisting of chlorotrifluoroethylene claim 2 , trifluoroethylene claim 2 , vinylidene fluoride claim 2 , vinyl fluoride claim 2 , ethylene claim 2 , propylene claim 2 , perfluoro(3-butenyl vinyl ether) claim 2 , a perfluoro(allyl vinyl ether) claim 2 , a perfluoro α-olefin claim 2 , a (perfluoroalkyl)ethylene claim 2 , a (perfluoroalkyl)propene claim 2 , a perfluoro(alkyl vinyl ether) and a perfluoromonomer having a 5-membered ring.4: A sulfonic acid containing polymer obtained by hydrolysis of the fluorosulfonyl groups of the fluorosulfonyl group-containing polymer of ; wherein an ion exchange capacity of the sulfonic acid containing polymer is from 0.5 to 2.5 meq/g dry resin.5: A sulfonic acid containing polymer obtained by hydrolysis of the fluorosulfonyl groups of the fluorosulfonyl group-containing polymer of ; wherein an ion exchange capacity of the sulfonic acid containing polymer is from 0.5 to 2.5 meq/g dry resin.6: A sulfonic acid containing polymer obtained by hydrolysis of the fluorosulfonyl groups of the fluorosulfonyl group-containing polymer of ; wherein an ion exchange capacity of the sulfonic acid containing polymer is from 0.5 to 2.5 meq/g dry resin. This application is a divisional application of prior U.S. application Ser. No. 16/801,222 filed Feb. 26, 2020, the disclosure of which is incorporated herein by reference in its entirety. U.S. application Ser. No. 16/801,222 is a ...

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Номер записи: 75
24-01-2019 дата публикации

METHOD FOR MAKING N-(FLUOROSULFONYL) DIMETHYLAMINE

Номер: US20190023653A1
Автор: JOHNSON Martin Reid
Принадлежит:

Dimethylamine (MeNH) is reacted with sulfuryl fluoride (SOF) to form at least a first phase comprising N-(fluorosulfonyl) dimethylamine (FSONMe), tetramethylsulfamide (SO(NMe)), or a combination thereof. A second phase, which may include dimethylamine hydrofluoride (MeNHF), may be also formed and separated from the first phase. FSONMeor SO(NMe)is then isolated from the first phase. For example, the first phase may be a liquid phase, and FSONMeand SO(NMe)are separated by distillation, optionally under reduced pressure. 1. A method , comprising:{'sub': 2', '2', '2', '2', '2', '2', '2', '2, 'reacting dimethylamine (MeNH) with sulfuryl fluoride (SOF) in a solvent comprising water to form at least a first phase being a liquid phase and comprising N-(fluorosulfonyl) dimethylamine (FSONMe), tetramethylsulfamide (SO(NMe)), or a mixture thereof; and'}{'sub': 2', '2', '2', '2', '2, 'isolating FSONMeor SO(NMe)from the first phase.'}2. The method of claim 1 , wherein the solvent is a mixture comprising water and a second solvent.3. The method of claim 2 , wherein the second solvent is selected from the group consisting of dichloromethane claim 2 , ethyl ether claim 2 , tetrahydrofuran claim 2 , 2-methyltetrahydrofuran claim 2 , methylcyclopentyl ether claim 2 , methyl tert-butyl ether claim 2 , acetonitrile claim 2 , propionitrile claim 2 , butyronitrile claim 2 , toluene claim 2 , and any combination thereof.4. The method of claim 1 , further comprising separating a second phase from the first phase claim 1 , wherein the second phase comprises dimethylamine hydrofluoride (MeNHF).5. The method of claim 4 , wherein the second phase is in a liquid form above the first phase or a solid form.6. The method of claim 1 , wherein FSONMeor SO(NMe)is isolated by distilling the first phase claim 1 , optionally under a reduced pressure.7. The method of claim 8 , further comprising separating FSONMeand SO(NMe).8. The method of claim 7 , wherein FSONMeis a resulting product having a yield of ...

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Номер записи: 76
28-01-2021 дата публикации

METHODS FOR PROMOTING MYELINATION AND FOR TREATING DEMYELINATING DISEASES

Номер: US20210023218A1
Автор: Beyer Brittney, Fang Mingliang, Lairson Luke, Siuzdak Gary
Принадлежит:

This invention provides novel methods for treating or ameliorating symptoms of demyelinating diseases such as multiple sclerosis. The methods involve administering to subjects in need of treatment a pharmaceutical composition that contains a therapeutically effective amount of taurine and also a compound that induces oligodendrocyte precursor cell (OPC) differentiation (e.g., T3, benztropine, clemastine or miconazole). Some of the methods additionally involve administration to the subject a known agent for treating demyelinating diseases (e.g., SIP receptor agonists) or a known disease modifying drug. The invention also provides methods for increasing myelination and methods for promoting OPC differentiation into oligodendrocytes. These methods entail contacting a population of OPCs with a combination of taurine and a known OPC differentiation-inducing agent such as T3, clemastine, benztropine or miconazole. 1. A method for treating or ameliorating one or more symptoms of a demyelinating disease in a subject , comprising administering to the subject (a) a pharmaceutical composition comprising a therapeutically effective amount of taurine or a taurine-like compound and (b) an agent that induces oligodendrocyte precursor cell (OPC) differentiation (OPC differentiation-inducing agent) , thereby treating or ameliorating the symptoms of the demyelinating disease in the subject.2. The method of claim 1 , wherein the taurine or taurine-like compound is administered to the subject simultaneously with claim 1 , prior to claim 1 , or subsequent to administration of the OPC differentiation-inducing agent.3. The method of claim 1 , wherein the taurine-like compound is an agent that can directly or indirectly upregulate the serine level in an OPC claim 1 , pre-myelinating oligodendrocyte claim 1 , or oligodendrocyte claim 1 , thereby enhancing glycosphingolipid biosynthesis in the OPC claim 1 , pre-myelinating oligodendrocyte claim 1 , or oligodendrocyte.4. The method of claim 1 ...

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Номер записи: 77
25-01-2018 дата публикации

MANUFACTURE OF A CHARGE DIRECTOR

Номер: US20180024456A1
Автор: Bachar Eyal, Kornilov Julia, Tchaicheeyan Hanit Marom, Teishev Albert
Принадлежит: HP INDIGO B.V.

Herein is described a method for the manufacture of a charge director comprising a barium salt. The method comprises reacting barium alkoxide with an acid in a reaction medium comprising ethanol, and separating ethanol from the reaction mixture to recover the barium salt produced. 1. A method for the manufacture of a charge director comprising a barium salt , said method comprising:reacting barium alkoxide with an acid in a reaction medium comprising ethanol, andseparating ethanol from the reaction mixture to recover the barium salt produced.2. A method as claimed in claim 1 , wherein the barium alkoxide is barium ethoxide.3. A method as claimed in any one of the preceding claims claim 1 , wherein the reaction between barium alkoxide with an acid occurs in the substantial absence of methanol.4. A method as claimed in any one of the preceding claims claim 1 , wherein the acid is selected from at least one of a sulfosuccinic acid alkyl ester and phosphoric acid.5. A method as claimed in claim 4 , wherein the acid comprises a sulfosuccinic acid alkyl ester and phosphoric acid.6. A method as claimed in or claim 4 , wherein the sulfosuccinic acid alkyl ester is an sulfosuccinic acid dialkyl ester.7. A method as claimed in claim 6 , wherein the barium salt comprises barium hydrogenphosphate and a barium salt of a sulfosuccinic acid dialkyl ester.9. A method as claimed in any one of to claim 6 , wherein the sulfosuccinic acid is provided as an ethanolic solution bydissolving an alkali metal salt of the sulfosuccinic acid alkyl ester in a first organic solvent,adding aqueous sulphuric acid to the solution to form the sulfosuccinic acid alkyl ester and alkali metal sulphate,removing alkali metal sulphate as an aqueous phase to leave an organic phase comprising the sulfosuccinic acid alkyl ester in the first organic solventextracting the sulfosuccinic acid alkyl ester from the first organic solvent by adding a second organic solvent to the organic phase,removing the first ...

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Номер записи: 78
23-01-2020 дата публикации

Carboxylate salt or sulfonate salt, and surfactant

Номер: US20200024219A1
Автор: Akiyoshi Yamauchi, Hirokazu Aoyama, Masahiro Higashi, Satoru Yoneda, Sumi Ishihara, Yosuke Kishikawa
Принадлежит: Daikin Industries Ltd

A carboxylic acid or sulfonic acid salt containing a plurality of carbonyl groups, and a surfactant represented by the following formula: R 1 —C(═O)—R 2 —C(═O)—R 3 -A wherein R 1 , R 2 and R 3 are as defined herein, and A is —COOX or —SO 3 X, wherein X is H, a metal atom, NR 4 4 , imidazolium optionally containing a substituent, pyridinium optionally containing a substituent, or phosphonium optionally containing a substituent, where R 4 s are each H or an organic group and are the same as or different from each other; and any two of R 1 , R 2 , and R 3 optionally bind to each other to form a ring.

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Номер записи: 79
23-01-2020 дата публикации

NEW METHOD FOR PRODUCING 2-ACRYLAMIDO-2-METHYLPROPANE SULPHONIC ACID

Номер: US20200024228A1
Автор: Favero Cédrick, KIEFFER Johann
Принадлежит: S.P.C.M. SA

The present invention relates to a production process for 2-acrylamido-2-methylpropane sulfonic acid including at least the following successive steps: 1. A production process for 2-acrylamido-2-methylpropane sulfonic acid including at least the following successive steps:{'sub': '3', '1) mixing of acrylonitrile with at least one compound contributing SOat a temperature included between −80 and 30° C. for at least one second in order to obtain a sulfonating mixture;'}{'sub': '3', '2) placing in contact and mixing isobutylene and the sulfonating mixture with a molar ratio of SOto isobutylene included between 0.2:1 and 2:1 and a molar ratio of acrylonitrile to isobutylene included between 3:1 and 60:1 at a temperature included between −40 and 100° C. for a time included between 10 seconds and 300 minutes in order to obtain a reaction mixture;'}3) solid/liquid separation of the reaction mixture and isolation of the solid particles contained in the reaction mixture in the form of a composition 1 in which the solid particles represent 50 to 99% by weight of the composition 1;4) mixing composition 1 at the end of step 3) with an aqueous solution A for at least 10 minutes at a temperature included between −20 and 70° C. in order to obtain a suspension 1 of 2-acrylamido-2-methylpropane sulfonic acid crystals;5) solid/liquid separation of the suspension 1 and isolation of the crystals in the form of a composition 2 in which the crystals represent between 40 and 99% by weight of the composition 2.2. The process according to claim 1 , wherein the compound contributing SOis fuming sulfuric acid claim 1 , used at a concentration included between 100% and 113.5%.3. The process according to claim 1 , wherein step 1) includes mixing acrylonitrile with at least one compound contributing SOin a solvent 1.4. The process according to claim 3 , wherein the solvent 1 is acrylonitrile.5. The process according to claim 1 , wherein isobutylene is added claim 1 , during step 2) claim 1 , ...

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Номер записи: 80
28-01-2021 дата публикации

Aminated lignin-derived compounds and uses thereof

Номер: US20210024453A1
Автор: Alexander Möller, Evgeny LARIONOV, Jan HARTWIG, Nastaran KRAWCZYK, Peter Geigle
Принадлежит: Cmblu Energy Ag, CMBLU PROJEKT AG

The present invention relates to novel lignin-derived compounds and compositions comprising the same and their use as redox flow battery electrolytes. The invention further provides a method for preparing said compounds and compositions as well as a redox flow battery comprising said compounds and compositions. Additionally, an assembly for carrying out the inventive method is provided.

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Номер записи: 81
25-01-2018 дата публикации

Carbazole-based gumbos for highly efficient blue oleds

Номер: US20180026201A1
Автор: Isiah Manuel Warner, Noureen Siraj, Thenahandi Prasanthi Deepthika De Silva
Принадлежит: Louisiana State University and Agricultural and Mechanical College

Various examples are provided for carbazole-based GUMBOS (group of uniform materials based on organic salts), and its application in organic light emitting diodes (OLEDs). In one example, a composition includes a solid phase carbazole-based GUMBOS (group of uniform materials based on organic salts) comprising a counterion such as, e.g., trifluoromethanesulfonate ([Otf]), bis-(trifluoromethanesulfonyl)imide ([NTf 2 ]), bis-(pentafluoroethylsulfonyl)imide ([BETI]), tetrafluoroborate (BF4), hexa-fluorophosphate (PF6), and/or thiocyanate (SCN). The carbazole-based GUMBOS can include carbazoleimidazole-based GUMBOS or 3,6-diBDC carbazolium-based GUMBOS. In another example, a method includes preparing a biphasic solution; separating a layer of DCM from the biphasic solution after stirring; washing the DCM with water to remove byproducts; and evaporating the DCM to form a solid phase carbazoleimidazole-based GUMBOS. Preparing the biphasic solution can include carbazoleimidazolium iodide (CM) dissolved in dichloromethane (DCM) and a dissolved salt including a sodium salt or a lithium salt.

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Номер записи: 82
04-02-2016 дата публикации

Minocycline Derivatives

Номер: US20160030452A1
Автор: KENNEDY JACK PHILLIP, Waugh Jacob M.
Принадлежит:

This invention relates generally to minocycline derivatives, and to compositions, including pharmaceutical compositions, containing such minocycline derivatives. The invention also relates to methods of synthesizing minocycline derivatives and to methods for using such minocycline derivatives as anti-bacterial agents for treating or preventing infections. 2. The compound according to claim 1 , wherein Ris alkyl.3. The compound according to claim 2 , wherein the alkyl comprises 1 to 20 carbon atoms.4. The compound according to claim 3 , wherein the alkyl comprises 1 to 10 carbon atoms.5. The compound according to claim 4 , wherein the alkyl comprises 1 to 5 carbon atoms.6. The compound according to claim 5 , wherein the alkyl comprises 1 to 3 carbon atoms.7. The compound according to claim 2 , wherein the alkyl is selected from the group consisting of methyl claim 2 , ethyl claim 2 , propan-1-yl claim 2 , propan-2-yl claim 2 , cyclopropan-1-yl; butan-1-yl claim 2 , butan-2-yl claim 2 , 2-methyl-propan-1-yl claim 2 , 2-methyl-propan-2-yl claim 2 , and cyclobutan-1-yl.8. The compound according to claim 7 , wherein the alkyl is methyl or ethyl.9. The compound according to claim 8 , wherein the alkyl is methyl.10. The compound according to claim 1 , wherein Ris a substituted alkyl.11. The compound according to claim 10 , wherein the substituted alkyl contains 1 to 20 carbon atoms.12. The compound according to claim 11 , wherein the substituted alkyl contains 1 to 15 carbon atoms.13. The compound according to claim 12 , wherein the substituted alkyl contains 1 to 10 carbon atoms.14. The compound according to claim 13 , wherein the substituted alkyl contains 1 to 5 carbon atoms.15. The compound according to claim 10 , wherein the substituted alkyl is selected from the group consisting of —X claim 10 , —CX claim 10 , —OR claim 10 , —C(O)R claim 10 , —C(S)R claim 10 , —C(O)OR claim 10 , —C(O)NRR claim 10 , —SR claim 10 , —S— claim 10 , ═S claim 10 , —O— claim 10 , ═O claim ...

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Номер записи: 83
04-02-2016 дата публикации

Poly-Perfluoroalkyl Substituted Polyethyleneimine Foam Stabilizers and Film Formers

Номер: US20160030793A1
Автор: XIE Yuan
Принадлежит:

Poly-perfluoroalkyl substituted polyethyleneimine compositions are provided that act as foam stabilizers and film formers when used in fire-fighting foam concentrates. The polyethylene compositions are soluble in water, but have only low solubility in polar solvents. When aqueous film forming foam generated from these concentrates is applied to burning polar solvent the polyethyleneimine compositions precipitate at the polar solvent/foam interface and inhibit the collapse and destruction of the foam. 1. A foam stabilizer comprising a highly branched substituted polyamine wherein the amino groups of said polyamine are substituted with:{'sub': 2', 'm', '2', 'n, '(a) —(CH)(CF)F, wherein m is 1-12 and n is 4-16; and'}{'sub': 2', 'p', '2', 'q', '3', '2', 'p', '2', 'q', '4', '2', 'p, 'sup': −', '+', '−, '(b) a hydrophilic moiety selected from the group consisting of —(CH)CHOH(CH)SO, (CH)CHOH(CH)NHand (CH)COO; wherein p and q independently are 1-6 and p+q is 2-8;'}{'sub': 'w', 'wherein said substituted polyamine has an average molecular weight Mof between about 5 kDa and 25 kDa prior to substitution; and'}wherein said stabilizer has a fluorine content of about 15 to about 25%.2. A foam stabilizer according to wherein said amino groups of said polyamine are further substituted with a siloxane moiety selected from the group consisting of (RSiO)Si(R)(CH)OCHCHOHCH— and RSiO[Si(R)O]Si(CH)OCHCHOHCH claim 1 , wherein each R independently is lower alkyl claim 1 , r=1-9 claim 1 , and wherein said stabilizer has a silicon content of about 0.1 to about 10%.3. A foam stabilizer according to wherein n is 4-6.4. A foam stabilizer according to wherein n is 6.5. A foam stabilizer according to wherein m is 1 or 2.6. A foam stabilizer according to wherein p and q are 1 or 2.7. A foam stabilizer according to wherein said siloxane moiety is (MeSiO)Si(Me)(CH)OCHCHOHCH— or CHSi(CH)O[Si(CH)O]Si(CH)OCHCHOHCH—.8. A foam stabilizer according to wherein the average molecular weight Mof the ...

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Номер записи: 84
24-04-2014 дата публикации

Process for Producing Fluorosulfuric Acid Aromatic-Ring Esters

Номер: US20140114088A1
Автор: Ishii Akihiro, Ishimaru Takehisa, Yamazaki Takako, YASUMOTO Manabu
Принадлежит: CENTRAL GLASS COMPANY, LIMITED

A production process of a fluorosulfuric acid aromatic-ring ester according to the present invention includes reaction of an aromatic-ring hydroxyl compound with sulfuryl fluoride (SOF) in the presence of a tertiary amine except pyridine and methylpyridine. The sulfuryl fluoride, used as the reactant in the production process according to the present invention, is widely adapted as a fumigant and is easily available on a large scale. Further, the target compound can be obtained rapidly with a high yield under moderate reaction conditions in the production process according to the present invention. In this way, all of the prior art problems can be solved in the production process according to the present invention. The production process according to the present invention is thus particularly useful for industrial production of the fluorosulfuric acid aromatic-ring ester. 2. The process according to claim 1 , wherein the reaction is conducted at a reaction temperature of 75° C. or lower.3. The process according to claim 1 , wherein the reaction is conducted at a reaction pressure of 1.0 MPa or lower.4. The process according to any one of claim 1 , wherein the reaction is conducted in a reaction time of 12 hours or less.5. The process according to claim 1 , wherein the tertiary amine is at least one selected from the group consisting of triethylamine claim 1 , diisopropylethylamine claim 1 , tri-n-propylamine claim 1 , tri-n-butylamine claim 1 , N-methylpiperidine claim 1 , 1-ethylpiperidine claim 1 , N claim 1 ,N-dicyclohexylmethylamine claim 1 , N claim 1 ,N-dicyclohexylethylamine claim 1 , 4-dimethylaminopyridine claim 1 , 1 claim 1 ,5-diazabicyclo[4.3.0]nona-5-ene and 1 claim 1 ,8-diazabicyclo[5.4.0]undec-7-ene.6. The process according to claim 1 , wherein claim 1 , as Ar claim 1 , the aromatic-ring group is an aromatic hydrocarbon or aromatic heterocyclic group of 1 to 18 carbon atoms and the substituted aromatic-ring group is an aromatic hydrocarbon or aromatic ...

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Номер записи: 85
01-02-2018 дата публикации

PROCESSES FOR FORMING TITANIUM CATECHOL COMPLEXES

Номер: US20180029965A1
Автор: MILLARD Matthew
Принадлежит:

Titanium complexes containing catecholate ligands can be desirable active materials for flow batteries and other electrochemical energy storage systems. Such complexes can be formed, potentially on very large scales, through reacting a catechol compound in an organic solvent with titanium tetrachloride, and then obtaining an aqueous phase containing an alkali metal salt form of the titanium catechol complex. More specifically, the methods can include: forming a catechol solution and heating, adding titanium tetrachloride to the catechol solution, reacting the titanium tetrachloride with a catechol compound to evolve HCl gas and to form an intermediate titanium catechol complex, and adding an alkaline aqueous solution to the intermediate titanium catechol complex to form an alkali metal salt form titanium catechol complex that is at least partially dissolved in an aqueous phase. The aqueous phase can be separated from an organic phase. The resulting complexes can be substantially free of alkali metal halide salts. 1. A method comprising:forming a catechol solution comprising a catechol compound and an organic solvent;heating the catechol solution;adding titanium tetrachloride to the catechol solution to form a reaction mixture;reacting the titanium tetrachloride with the catechol compound to evolve HCl gas from the reaction mixture and to form an intermediate titanium catechol complex; and 'wherein the alkali metal base converts the intermediate titanium catechol complex into an alkali metal salt form titanium catechol complex that is at least partially dissolved in an aqueous phase.', 'adding an alkaline aqueous solution to the intermediate titanium catechol complex, the alkaline aqueous solution comprising an alkali metal base;'}2. The method of claim 1 , wherein the catechol compound is 1 claim 1 ,2-dihydroxybenzene.3. The method of claim 1 , wherein the catechol compound comprises at least one substituted catechol compound.4. The method of claim 3 , wherein the ...

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Номер записи: 86
17-02-2022 дата публикации

SYNTHETIC PROCESS

Номер: US20220048859A1
Автор: Bondigela Siva Sankar, Coombs John Ryan, Gallagher William P., González-Bobes Francisco, Guerrero Carlos A., Joe Candice Lee, Kalidindi Srinivas, Kandasamy Moorthy, Kuppusamy Sankar, Marcoux David, Rupasinghe Sanjeewa, SHI Qing, Shunmugaraj Sathasivam, Tendulkar Shankar Tulsidas, Vaidyanathan Rajappa, Zhu Jason J.
Принадлежит:

The invention generally relates to a process for preparing compounds, including Compound of Formula (I), useful as key intermediates in the preparation of compounds having RORγt antagonist properties. 2. The process according to claim 1 , comprising the steps of(a) reacting Compound 1 with 4-fluorobenzenesulfinic acid in the presence of 1-methyl-2-pyrrolidinone and iodine to afford Compound 2,(b) reacting Compound 2 with heptafluoroisopropyl iodide in the presence of a base to afford Compound 3,(c) reducing Compound 3 with sodium borohydride in solvent to afford Compound 4,(d) reacting Compound 4 with trifluoroacetic anhydride and sodium t-pentoxide in the presence of 2-methyltetrahydrofuran to afford Compound 5,(e) reacting Compound 5 with Compound 6 in the presence of sodium t-pentoxide to afford Compound 7, and(f) reacting Compound 7 with chlorotrimethylsilane, followed by L-(+)-tartaric acid to afford the Compound of Formula (I).4. The process according to claim 3 , comprising the steps of(a) reacting Compound 8 with Compound 6 in the presence of sodium t-pentoxide and tetrahydrofuran to afford Compound 9.(b) reacting Compound 9 with chlorotrimethylsilane in the presence of a suitable solvent to afford Compound 10,{'sub': 2', '3, '(c) reacting Compound 10 with di-tert-butyl dicarbonate (BocO) in the presence of a NaHCOto afford Compound 11,'}{'sub': '2', '(d) reacting Compound 11 with iPrMgCl in the presence of COand tetrahydrofuran to afford Compound 12,'}(e) reacting Compound 12 with trifluoromethyltrimethylsilane and N,N′-carbonyldiimidazole in the presence of dichloromethane to obtain Compound 13, reacting Compound 13 with (diethylamino) difluorosulfonium tetrafluoroborate in dichloromethane in the presence of tetrabutylammonium fluoride (TBAF) or cesium fluoride (CsF) to obtain Compound 14, and(g) reacting Compound 14 with HCl in dioxane to obtain the Compound of Formula (II).6. The process according to claim 5 , comprising the steps of(a) converting ...

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Номер записи: 87
30-01-2020 дата публикации

METHOD FOR PREPARING (R)-N-[4-(1-AMINO-ETHYL)-2,6-DIFLUORO-PHENYL]-METHANESULFONAMIDE

Номер: US20200031766A1
Автор: CHOI Chang Soon, JAYAPRAKASH Sarva, LEE Jihae, LEE Ki-Wha, PARK Miyoung, PARK Young-ho, PATEL Krushnakant, RAMAMOHAN M., REGATI Sridhar, SRINIVAS Mamidi, WOO Byoung young
Принадлежит: AMOREPACIFIC CORPORATION

Disclosed in the present specification is a method capable of preparing N-[4-[(1R)-1-[[(R)-(1,1-dimethylethyl)sulfinyl]amino]ethyl]-2,6-difluorophenyl]-methanesulfonamide (INT028-2) with high optical purity, through the selection of Ellman-chiral auxiliaries and the re-crystallization and separation of optical isomers. According to the above method, high-purity N-[4-[(1R)-1-[[(R)-(1,1-dimethylethyl)sulfinyl]amino]ethyl]-2,6-difluorophenyl]-methanesulfonamide with excellent quality can be produced at room temperature by improving cryogenic process conditions necessary for realizing high optical purity, and thus the trimming due to the process failure rate can be remarkably reduced. 1. A method for preparing (R)—N-[4-(1-aminoethyl)-2 ,6-difluoro-phenyl]-methanesulfonamide , the method comprising:a recrystallization step including putting and stirring a stereoisomeric mixture in which optical isomers of N-[4-[(1R)-1-[[(R)-(1,1-dimethylethyl)sulfinyl]amino]ethyl]-2,6-difluorophenyl]-methanesulfonamide are mixed in a specific solvent and obtaining a solid which is precipitated in a solution phase and contains N-[4-[(1R)-1-[[(R)-(1,1-dimethylethyl)sulfinyl]amino]ethyl]-2,6-difluorophenyl]-methanesulfonamide, whereinthe solvent in the recrystallization step includes one or more kinds selected from the group consisting of isopropyl alcohol (IPA), methanol (MeOH), ethyl acetate (EtOAc), toluene, and isopropyl acetate.2. The method for preparing (R)—N-[4-(1-aminoethyl)-2 claim 1 ,6-difluoro-phenyl]-methanesulfonamide according to claim 1 , wherein the solvent in the recrystallization step is selected from the group consisting of isopropyl alcohol (IPA) claim 1 , methanol:ethyl acetate (MeOH:EtOAc) (1:8) claim 1 , methanol:ethyl acetate (1:6) claim 1 , ethyl acetate (EtOAc) claim 1 , ethyl acetate:toluene (1:2) claim 1 , ethyl acetate:toluene (1:1) claim 1 , and isopropyl acetate.3. The method for preparing (R)—N-[4-(1-aminoethyl)-2 claim 1 ,6-difluoro-phenyl]- ...

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Номер записи: 88
04-02-2021 дата публикации

Radical initiators and chain extenders for converting methane gas into methane-sulfonic acid

Номер: US20210032200A1
Автор: Alan K. Richards
Принадлежит: Veolia North America Regeneration Services LLC

Improved initiators, solvents, and SO3 mixtures are disclosed herein, which can increase the yields and efficiency of a chemical manufacturing process which uses a radical chain reaction to convert methane (CH4), which is a gas under any normal conditions, into methane-sulfonic acid (MSA), a liquid. MSA is useful and valuable in its own right, and it also can be processed to create desulfured fuels and other valuable chemicals. A preferred initiator combination has been identified, comprising at least two different sulfate peroxide compounds. One type or class of initiator can be called a “primary” (or major, main, principle, dominant, or similar terms) initiator, and the other type or class of initiator can be can be regarded as an “extender” (or secondary, supplemental, enhancing, tuning, tweaking, or similar terms) initiator. “Primary” initiator(s) include (unmethylated) Marshall's acid, mono-methyl-Marshall's acid, and di-methyl-Marshall's acid, while a secondary/extender initiator comprises methyl-Caro's acid, which can oxidize sulfur DI-oxide (an unwanted chain terminator) into sulfur TRI-oxide (an essential reagent). Various other enhancements to the MSA manufacturing process also are described.

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Номер записи: 89
05-02-2015 дата публикации

Transcription Factor Inhibitors and Related Compositions, Formulations and Methods

Номер: US20150038443A1
Автор: Li Chenglong, Li Pui-Kai, Lin Jiayuh
Принадлежит:

The present invention provides small molecules useful to affect cancer cells, along with related methods. The present compounds, formulations, kits and methods are useful for a variety of research, diagnostic and therapeutic purposes. STAT3 inhibitors, particularly LLL12, are disclosed. The STAT3 inhibitors are useful to treat breast cancer in general and breast cancer initiating cells in particular. 2. A composition of matter claim 1 , comprising a compound of and a pharmaceutically-acceptable excipient claim 1 , carrier claim 1 , diluents claim 1 , or salt.3. A method to synthesize a compound of claim 1 , comprising:i) reacting an unsubstituted or substituted naphthalene sulfonyl chloride compound with a nitrogen containing compound to form an unsubstituted or substituted naphthalene sulfonyl amine;ii) oxidizing the unsubstituted or substituted naphthalene sulfonyl amine of step i) to yield an unsubstituted or substituted naphthoquinone compound; andiii) catalyzing via a Diels-Alder reaction of 3-hydroxy-2-pyrone with the unsubstituted or substituted naphthoquinone compound of step ii) to yield a compound of formula I.4. The method of claim 3 , wherein the nitrogen containing compound of step i) comprises ammonium hydroxide and the naphthalene sulfonyl chloride is unsubstituted.5. A method to inhibit STAT3 activation in a cell claim 1 , comprising introducing a compound of to a STAT3-expressing cell claim 1 , and measuring STAT3 activation inhibition.6. The method of claim 5 , wherein said inhibition is measured by observing cell apoptosis.7. The method of claim 5 , wherein said inhibition is measured by observing prevention of STAT3 SH2 dimerization.8. The method of claim 5 , wherein said inhibition is measured by observing a decrease in the levels of expression of STAT3 phosphorylation.9. The method of claim 5 , wherein said inhibition is measured by observing inhibition of downstream targets of STAT3.10. The method of claim 9 , wherein said downstream targets ...

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Номер записи: 90
08-02-2018 дата публикации

METHOD FOR PRODUCING OXYSULPHIDIC AND FLUORINATED DERIVATIVES IN AN IONIC LIQUID MEDIUM

Номер: US20180037543A1
Автор: METZ François
Принадлежит:

The invention relates to a method for producing an oxysulphidic and fluorinated derivative in the form of a salt of formula (II) Ea-SOQ (II) comprising providing an ionic liquid compound of formula (I) in the liquid state Ea-SOOCr (II)—Ea representing the fluorine atom or a group having between 1 and 10 carbon atoms selected from fluoroalkyls, perfluoroalkyls and fluoroalkenyls; and—Q representing an onium cation, with a sulphur oxide, said ionic liquid compound of formula (I) representing at least 50 wt. % of the initial liquid reactive medium. 2. The process as claimed in claim 1 , in which the reaction medium is devoid of organic solvent of amide type.3. The process as claimed in claim 1 , in which the onium cation Qis selected from the group consisting of ammonium claim 1 , phosphonium claim 1 , pyridinium claim 1 , pyrazolinium claim 1 , imidazolium claim 1 , arsenium claim 1 , quaternary ammonium and quaternary phosphonium cations.4. The process as claimed in claim 1 , in which the onium cation Qis a quaternary phosphonium cation.5. The process as claimed in claim 1 , in which the cation Qrepresents a quaternary ammonium cation selected from the group consisting of tetraethylammonium claim 1 , tetrapropylammonium claim 1 , tetrabutylammonium claim 1 , trimethylbenzylammonium claim 1 , methyltributylammonium and Aliquat 336.6. The process as claimed in claim 1 , in which the cation Qrepresents a pyridinium cation.7. The process as claimed in claim 1 , for the preparation of a trifluoromethanesulfinic acid onium salt CF SOOQ.8. The process as claimed in claim 7 , in which the trifluoromethanesulfinic acid onium salt CFSOOQis tetrabutylphosphonium trifluoromethanesulfinate CFSOOPBu.9. A process for the preparation of a compound in the form of a salt of formula (III):{'br': None, 'sub': '3', 'sup': −', '+, 'Ea-SOQ\u2003\u2003(III)'}Ea representing a fluorine atom or a group having from 1 to 10 carbon atoms selected from the group consisting of fluoroalkyls, ...

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Номер записи: 91
08-02-2018 дата публикации

SYNTHESIS OF SULFUR CONTAINING AMMONIUM AND PHOSPHONIUM BORATES

Номер: US20180037558A1
Автор: HERBEL Juergen, HOLUB Nicole
Принадлежит: BASF SE

The present invention relates to the preparation of sulfur containing ammonium and phosphonium borates KA wherein K is a compound of formula (I) A is an anion of formulae (IIa) or (IIb) by bringing into contact ammonium borates with sulfur containing ammonium or phosphonium halides or sulfonates 2. The process according to claim 1 , wherein X is N.3. The process according to claim 1 , wherein Rand Rare linked and jointly selected from —(CH)— alkylene with m=4 or 5 forming together with the central X-atom a five- or six-membered heterocycle wherein one or more H of —(CH)— alkylene may be replaced by one or more substituents selected from F and optionally fluorinated C-Calkyl claim 1 , and wherein one or more CHgroups of —(CH)— alkylene may be replaced by O claim 1 , S or NR′.4. The process according to claim 1 , wherein A is selected from bis(oxalato) borate and difluoro oxalato borate.5. The process according to claim 1 , wherein R claim 1 , R claim 1 , and Rare same and selected from C-Calkyl or Rand Rare linked and jointly selected from —(CH)— alkylene forming together with the central N-atom a five-membered saturated or aromatic heterocycle wherein one or more H of —(CH)— alkylene may be replaced by one or more substituents selected from C-Calkyl claim 1 , and wherein one or more CHgroups of —(CH)— alkylene may be replaced by O claim 1 , N or NR″ with R″ is selected from C-Calkyl and Ris selected from Cto Calkyl.6. The process according to claim 1 , wherein Ais an anion selected from [R—SO] and Rand Rare same.7. The process according to claim 1 , wherein the solvent or solvent mixture (i) is selected from Cto Calcohols claim 1 , di-Cto Calkylethers claim 1 , Cto Ccarboxylic acids claim 1 , Cto Calkylesters claim 1 , di-Cto Calkyl carbonates claim 1 , acetonitrile claim 1 , and Cto Cketones claim 1 , and mixtures thereof.8. The process according to claim 1 , wherein in step (b) a solution of KA′ in a first solvent or solvent mixture (i) is brought into contact ...

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Номер записи: 92
12-02-2015 дата публикации

METHOD FOR PREPARING FLUORINE-18 ELUENT WITH ADJUSTED PH, AND METHOD FOR LABELLING FLUORINE-18 USING SAME

Номер: US20150045548A1
Автор: Kim Jae Seung, LEE Jong Jin, LEE Sang Ju, Moon Dae Hyuk, Oh Seung Jun, Ryu Jin Sook
Принадлежит:

The present invention relates to a method for labelling fluorine-18, which is a radioisotope, and more specifically, to a method for labelling a [F]fluoride in a method for preparing an organic [F]fluoro compound by reacting an alkyl halide or an alkyl sulfonate with a [F]fluoride, wherein a [F]fluoride supported on a quaternary alkyl ammonium polymer support is eluted using a solution containing a metal salt or a quaternary ammonium salt with an adjusted pH, and a base is not additionally used. The present invention enables a labeling reaction without an additional base after precisely reflecting the concentration of a base absolutely necessary for the nucleophilic substitution of a [F]fluoride or eluting a [F]fluoride using a [F]fluoride eluent with an adjusted pH, thereby stably obtaining a [F]fluoride-labelled compound in a high yield, and is thus useful for production of fluorine-18-labelled radioactive medical supplies. 2. The method of claim 1 , wherein the alkyl group of Formula 1 is any one selected from the group consisting of a methyl group claim 1 , an ethyl group claim 1 , an isopropyl group claim 1 , a chloromethyl group claim 1 , a trifluoromethyl group claim 1 , and a chloroethyl group.3. The method of claim 1 , wherein the aryl group of Formula 1 is any one selected from the group consisting of a methylphenyl group claim 1 , an ethylphenyl group claim 1 , a chlorophenyl group claim 1 , a bromophenyl group claim 1 , a methoxyphenyl group claim 1 , and a nitrophenyl group.4. The method of claim 1 , wherein the ammonium of Formula 2 is selected from the group consisting of tetrabutylammonium claim 1 , benzyltrimethylammonium claim 1 , triethylammonium claim 1 , tributylammonium claim 1 , dibutylammonium claim 1 , dihexylammonium claim 1 , butylammonium claim 1 , and hexylammonium.5. An eluent of [F]fluoride prepared by the method of claim 1 , the eluent having a pH of 6-8 claim 1 , containing a metal salt or quaternary ammonium salt claim 1 , and ...

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Номер записи: 93
12-02-2015 дата публикации

NOVEL FUSED NAPHTHALENE CYCLOHETERO RING COMPOUNDS, AND METHODS AND USES THEREOF

Номер: US20150045560A1
Автор: He Mingqian, Hu Jieyu, Niu Weijun, Tandia Adama
Принадлежит:

Described herein are heterocyclic organic compounds of following formulae: More specifically, described herein are fused heterocyclic naphthalene compounds, polymers based on fused heterocyclic naphthalene compounds, methods for making these compounds, and uses thereof. The compounds described have improved polymerization and stability properties that allow for improved material processibility for use as organic semiconductors (OSCs). 2. The compound of claim 1 , wherein the compound is 1a or 1b.3. The compound of claim 1 , wherein the compound is 2a claim 1 , 2b claim 1 , or 2c.4. The compound of claim 1 , wherein:{'sub': 1', '1', '1', '1', '1', '1', '1, 'Xis S, Se, NR, PR, AsR, SbR, O, or Te, with the proviso that due to conjugation, Xmay be bonded to one or more additional R;'}{'sub': 2', '1', '2', '1, 'Xis N or CR, with the proviso that due to conjugation, Xmay be bonded to one or more additional R;'}{'sub': 1', '40', '2', '40', '2', '40', '3', '2', '2, 'y is H, halo, trialkylsiane, optionally substituted C-Calkyl, optionally substituted C-Calkenyl, optionally substituted C-Calkynyl, halo, OSO-alkyl, Mg-halo, Zn-halo, Sn(alkyl), B(OH), or B(alkoxy); and'}{'sub': 1', '1', '40', '2', '40', '2', '40, 'each Ris independently H, halo, optionally substituted C-Calkyl, optionally substituted aralkyl, alkoxy, alkylthio, optionally substituted C-Calkenyl, optionally substituted C-Calkynyl, aminocarbonyl, acylamino, acyloxy, optionally substituted aryl, aryloxy, optionally substituted amino, carboxyalkyl, optionally substituted cycloalkyl, optionally substituted cycloalkenyl, halo, acyl, optionally substituted heteroaryl, optionally substituted heteroaralkyl, heteroaryloxy, optionally substituted heterocyclyl, thiol, alkylthio, heteroarylthiol, optionally substituted sulfoxide, or optionally substituted sulfone.'}5. The compound of claim 4 , wherein each Ris independently H claim 4 , halo claim 4 , optionally substituted C-Calkyl claim 4 , optionally substituted aralkyl ...

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Номер записи: 94
06-02-2020 дата публикации

PROCESSES AND SYSTEMS FOR RECOVERING METHANESULFONIC ACID IN PURIFIED FORM

Номер: US20200039926A1
Автор: FORTMAN George C., MILLER Jay F., SMITH Gary S., SRINIVAS Vijay R.
Принадлежит:

Aspects of the invention relate to systems and processes for recovering methanesulfonic acid, in a purified form, from a composition additionally including sulfur trioxide. In accordance with one aspect, the invention provides a process that includes separating a feed stream comprised of hydrocarbons, methanesulfonic acid, sulfur trioxide, and optionally sulfuric acid to produce a light stream comprised of hydrocarbons and a heavy stream comprised of methanesulfonic acid and sulfur trioxide; contacting (e.g., by mixing) the heavy stream with a reactive additive capable of reacting with sulfur trioxide, under conditions effective to cause reaction of the reactive additive with the sulfur trioxide to produce a heavy reaction product having a boiling point higher than the boiling point of methanesulfonic acid; and separating the heavy stream using a distillation column to produce a distillate stream consisting essentially of methanesulfonic acid and a bottoms stream comprising the heavy reaction product. 1. A process for recovering anhydrous methanesulfonic acid , in a purified form , from a feed stream comprised of hydrocarbon , methanesulfonic acid and sulfur trioxide comprisiug:separating the feed stream to produce a light stream comprised of hydrocarbons and a heavy stream comprised of methanesulfonic acid and sulfur trioxide;contacting the heavy stream with a reactive additive capable of reacting with sulfur trioxide under conditions effective to cause reaction of the reactive additive with the sulfur trioxide to produce a heavy reaction product having a boiling point higher than the boiling point of sulfur trioxide; andseparating the heavy stream using a distillation column to produce a distillate stream consisting essentially of methanesulfonic acid and a bottoms stream comprising the heavy reaction product.2. The process of claim 1 , wherein separating the heavy stream further comprises recovering a stream consisting essentially of hydrocarbons using a vapor- ...

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Номер записи: 95
06-02-2020 дата публикации

PROCESS FOR PURIFYING ALKANESULFONIC ANHYDRIDE AND PROCESS FOR PRODUCING ALKANESULFONIC ACID USING THE PURIFIED ALKANESULFONIC ANHYDRIDE

Номер: US20200039927A1
Автор: FEDERSEL Katharina, RUETHER Feelly, SPIELMANN Jan, WORTMANN Jüergen
Принадлежит: BASF SE

A process for purifying alkanesulfonic anhydride which includes: 1. A process for purifying alkanesulfonic anhydride , comprising:(a) feeding a stream comprising alkanesulfonic anhydride, sulfuric acid, high boilers and residual low boilers into a melt crystallization to form crystals of the alkanesulfonic anhydride suspended in mother liquor;(b) performing a solid-liquid separation to remove the crystals from the mother liquor; and(c) optionally washing the crystals to remove mother liquor adhering to the crystals.2. The process according to claim 1 , wherein before feeding the stream comprising alkanesulfonic anhydride claim 1 , sulfuric acid claim 1 , high boilers and residual low boilers into the melt crystallization claim 1 , a distillation for removing low boilers is carried out.3. The process according to claim 2 , wherein a crude product stream is fed into a distillation apparatus claim 2 , the crude product stream comprising alkanesulfonic anhydride claim 2 , sulfuric acid claim 2 , high boilers and low boilers.4. The process according to claim 1 , wherein the mother liquor after removal of the crystals in (b) and/or the mother liquor generated in (a) is at least partly recycled into the melt crystallization.5. The process according to claim 1 , wherein the low boilers comprise sulfur trioxide.6. The process according to claim 1 , wherein the melt crystallization is carried out at a temperature in the range from 0 to 70° C.7. The process according to claim 1 , wherein the crystals are washed with molten crystallizate in (c).8. The process according to claim 7 , wherein the molten crystallizate for washing the crystals has a temperature 0.1° C. to 15° C. above the solidification temperature of the alkanesulfonic-anhydride-containing crystallizate.9. The process according to claim 1 , wherein the alkanesulfonic anhydride is methanesulfonic anhydride.10. A process for producing and purifying alkanesulfonic anhydride comprising:(i) optionally distilling a melt ...

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Номер записи: 96
18-02-2016 дата публикации

VINYL-GROUP-CONTAINING FLUORENE COMPOUND

Номер: US20160046551A1
Автор: AKAI Yasuyuki, Chisaka Hiroki, KITAO Kyuhei, NARASAKI Yoshiya, Noda Kunihiro, Shiota Dai, Takase Ichiro, TANIDA Daisuke
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A novel vinyl-group-containing fluorene compound and a method for producing the same, a polymerizable monomer and cross-linking agent including this compound, a leaving-group-containing fluorene compound, a monovinyl-group-containing fluorene compound, and methods for producing the same. This vinyl-group-containing fluorene compound is represented by formula (1). In the formula, Wand Wrepresent a group represented by formula (2), a group represented by formula (4), a hydroxyl group, or a (meth)acryloyloxy group, Rand Rrepresent a cyano group, a halogen atom, or a monovalent hydrocarbon, and n1 and n2 are integers of 0-4. In formulas (2) and (4), a ring (Z) is an aromatic hydrocarbon ring, X is a single bond or a group represented by —S—, Ris a single bond or a C1-4 alkylene group, Ris a specific substituent group such as a monovalent hydrocarbon, and m is an integer of 0 or greater. 2. The vinyl-group-containing fluorene-based compound according to claim 1 , wherein the ring Z is a benzene ring or a naphthalene ring.3. (canceled)4. A polymerizable monomer comprising the vinyl-group-containing fluorene-based compound according to .5. A crosslinking agent comprising the vinyl-group-containing fluorene-based compound according to wherein Wand Weach are independently the group represented by the general formula (2) or a (meth)acryloyloxy group.7. The process for producing a vinyl-group-containing fluorene-based compound according to claim 6 , wherein the ring Z is a benzene ring or a naphthalene ring.8. (canceled)10. The leaving group-containing fluorene-based compound according to claim 9 , wherein the ring Z is a benzene ring or a naphthalene ring.11. (canceled)13. The process for producing a vinyl-group-containing fluorene-based compound according to claim 12 , wherein the ring Z is a benzene ring or a naphthalene ring.14. (canceled)16. The process for producing a monovinyl-group-containing fluorene-based compound according to claim 15 , wherein the ring Z is a ...

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Номер записи: 97
18-02-2016 дата публикации

DIARYLIODONIUM SALT

Номер: US20160046566A1
Автор: MATSUZAKI Kohei, OKUYAMA Kenta, Saito Norimichi, SHIBATA Norio
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Provided is a compound that allows easy introduction of a pentafluorosulfanylaryl group into a compound of interest. 2. The diaryliodonium salt according to claim 1 , wherein m is 0 claim 1 , and n is 3.3. The diaryliodonium salt according to claim 2 , wherein Ris a methyl group claim 2 , an ethyl group claim 2 , a n-propyl group claim 2 , or an i-propyl group.4. The diaryliodonium salt according to claim 1 , wherein m is 0 claim 1 , and n is 0.7. The process according to claim 6 , wherein the nucleophilic compound Z is selected from the group consisting of a 1 claim 6 ,3-dicarbonyl compound claim 6 , a phenol compound claim 6 , an aniline compound claim 6 , a heterocyclic compound claim 6 , an alcohol compound claim 6 , an oxyimide compound claim 6 , an aromatic sulfur compound claim 6 , and an aromatic cyanogen compound. The present invention relates to a diaryliodonium salt. More particularly, this invention relates to a diaryliodonium salt and a process for introducing an aryl group containing a pentafluorosulfanyl group into a compound through the use of said diaryliodonium salt.The pentafluorosulfanyl (SF) group is known to exhibit a strong electron-withdrawing property due to the presence of fluorine atoms, and also to have high lipophilicity. Thus, compounds containing a SFgroup are expected to be applied to physiologically active substances such as liquid crystal materials and pharmaceutical and agricultural chemicals. However, a process for introducing a SFgroup into a compound of interest is not easy to carry out since this process uses chlorine gas or the like and so requires sophisticated equipment and skilled techniques. Thus, there has hitherto been reported a process for synthesizing a biaryl compound containing a SFgroup by subjecting an aromatic compound containing a SFgroup to coupling reaction in the presence of a transition metal catalyst (Non-patent Literature 1).However, there has been a need for a simpler process for introducing a SFgroup ...

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Номер записи: 98
18-02-2016 дата публикации

METHOD FOR THE PREPARATION OF (3S,3S') 4,4'-DISULFANEDIYLBIS (3-AMINOBUTANE 1-SULFONIC ACID)

Номер: US20160046571A1
Автор: Balavoine Fabrice, Cartigny Yohann, Coquerel Gerard, Couvrat Nicolas, Madec Jonathan, Petit Marie-Noelle, Schneider Jean-Marie
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The present invention relates to a new method for the preparation of (3S,3S′) 4,4′-disulfanediylbis(3-aminobutane 1-sulfonic acid) in five steps from (S)-ethyl 2-(benzyloxycarbonylamino)-4-(neopentyloxysulfonyl)butanoate A. 1. A trihydrate form of (3S ,3S′) 4 ,4′-disulfanediylbis(3-aminobutane 1-sulfonic acid).2. A trihydrate form of (3S ,3S′) 4 ,4′-disulfanediylbis(3-aminobutane 1-sulfonic acid) formed from (3S ,3S′) neopentyl 4 ,4′-disulfanediylbis(3-(benzyloxycarbonylamino)butane 1-sulfonate).3. A trihydrate form of (3S ,3S′) 4 ,4′-disulfanediylbis(3-aminobutane 1-sulfonic acid) formed from (S) ethyl 2-(benzyloxycarbonylamino) 4-(neopentyloxysulfonyl)butanoate4. A crystalline (3S ,3S′) 4 ,4′-disulfanediylbis(3-aminobutane 1-sulfonic acid)trihydrate , which has a powder XRD diffractogram with characteristic peaks at approximately: 5.09; 14.30; 15.30; 18.32 degrees 2θ (K_alpha1 Cu anode).5. A crystalline (3S ,3S′) 4 ,4′-disulfanediylbis(3-aminobutane 1-sulfonic acid)trihydrate , which has a powder XRD diffractogram with characteristic peaks at approximately: 5.09; 14.30; 15.30; 18.32; 22.09; 22.79; 24.65; 25.60 and 25.83 degrees 2θ (K_alpha1 Cu anode).6. A crystalline (3S ,3S′) 4 ,4′-disulfanediylbis(3-aminobutane 1-sulfonic acid)trihydrate , which has a powder XRD diffractorgram as essentially depicted in .8. The trihydrate of prepared according to a method comprising the steps of:(a) reducing the ethyl ester of (3S,3S′) 4,4′-disulfanediylbis(3-aminobutane 1-sulfonic acid) from (S) ethyl 2-(benzyloxycarbonylamino) 4-(neopentyloxysulfonyl)butanoate to give (S) neopentyl 3-(benzyloxycarbonylamino) 4-hydroxybutane 1-sulfonate B;(b) reacting the alcohol B with methanesulfonic anhydride or methanesulfonyl chloride in presence of a base to give (S) neopentyl 3-(benzyloxycarbonylamino) 4-(methylsulfonyloxy)butane 1-sulfonate C;(c) reacting the mesylated alcohol C with potassium thioacetate to give (S) 2-(benzyloxycarbonylamino) 4-(neopentyloxysulfonyl)butyl thioacetate D ...

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Номер записи: 99
01-05-2014 дата публикации

PROCESS FOR PRODUCING TAURINE

Номер: US20140121405A1
Автор: Chen Yong
Принадлежит: QIANJIANG YONGAN PHARMACEUTICAL CO., LTD

The present disclosure provides a process for producing taurine, includes: adjusting a PH value of a sodium taurate solution by a Scompound; introducing ethylene oxide into the sodium taurate solution to produce sodium hydroxyethyl sulfonate; separating crude taurine before or after introducing the ethylene oxide to the solution; and adding ammonia to the sodium hydroxyethyl sulfonate reaction solution to be reacted with the reaction solution to reproduce sodium taurate. The process for producing taurine of the present disclosure makes use of the balances of the sodium bases in the system, recycles the mother liquor until the sodium taurate is reproduced out of the reactions in the mother liquor, and thus is capable of allowing taurine to be synthesized and extracted. 1. A process for producing taurine , comprising:{'sup': '4+', '(1) adjusting a PH value of a sodium taurate solution by a Scompound;'}(2) introducing ethylene oxide into the sodium taurate solution to produce sodium hydroxyethyl sulfonate;(3) separating crude taurine before or after introducing the ethylene oxide to the solution; and(4) adding ammonia to the sodium hydroxyethyl sulfonate reaction solution to be reacted with the reaction solution to reproduce the sodium taurate.2. The process for producing taurine as claimed in claim 1 , wherein a concentration of the sodium taurate solution ranges from 45% to 48% by weight percentage before the PH value is adjusted in the step (1).3. The process for producing taurine as claimed in claim 1 , wherein the S compound used for adjusting the PH value in the step of (1) is SOor HSO.4. The process for producing taurine as claimed in claim 1 , wherein the PH value is adjusted to range from 4.5 to 9.0 by SOin the step (1).5. The process for producing taurine as claimed in claim 4 , wherein the PH value is adjusted to range from 5.5 to 6.5 by SOin the step (1).6. The process for producing taurine as claimed in claim 5 , wherein a concentration of the sodium ...

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Номер записи: 100