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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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Форма поиска

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 19852. Отображено 100.
23-02-2012 дата публикации

Method for producing color-stable mda and mdi

Номер: US20120046497A1
Принадлежит: BASF SE

The invention relates to a process for preparing methylenediphenyldiamine (MDA) by reacting formaldehyde and aniline in the presence of an acidic catalyst, wherein the oxygen content in the process for preparing MDA is <10 000 ppm, based on all compounds present in the process. The invention further relates to the phosgenation of MDA to methylenediphenyl diisocyanate (MDI).

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15-03-2012 дата публикации

Impactor ring for updraft classifiers

Номер: US20120061497A1
Автор: Rickey E. Wark
Принадлежит: Individual

An annular impactor structure for use in crusher/classifiers of the updraft type. An annular structure comprising a plurality of radially inwardly projecting, essentially vertical impactor plates of high-hardness material is located immediately above a vane structure such that entrained particulate matter from a milling bowl impacts one or both of the impactor plate surfaces. The impactor plates as well as the backer structures between the impactor plates are covered with coin-shaped protrusions. The impactor plate structure can be used in combination with a single or double course vane structure.

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03-05-2012 дата публикации

Method for the direct amination of hydrocarbons into amino hydrocarbons, including electrochemical separation of hydrogen and electrochemical reaction of the hydrogen into water

Номер: US20120107707A1
Принадлежит: BASF SE

Process for the direct amination of hydrocarbons to aminohydrocarbons by reaction of a feed stream E comprising at least one hydrocarbon and at least one aminating reagent to form a reaction mixture R comprising aminohydrocarbon and hydrogen in a reaction zone RZ and electrochemical separation of at least part of the hydrogen formed in the reaction from the reaction mixture R by means of a gastight membrane-electrode assembly having at least one selectively proton-conducting membrane and at least one electrode catalyst on each side of the membrane, where at least part of the hydrogen is oxidized to protons at the anode catalyst on the retentate side of the membrane and the protons pass through the membrane and on the permeate side are reacted with oxygen to form water, where the oxygen originates from an oxygen-comprising stream O which is brought into contact with the permeate side of the membrane, over the cathode catalyst.

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10-05-2012 дата публикации

Method for direct amination of hydrocarbons to form amino hydrocarbons with the electrochemical separation of hydrocarbon

Номер: US20120111732A1
Принадлежит: BASF SE

Process for the direct amination of hydrocarbons to aminohydrocarbons, which comprises the steps: a) reaction of a feed stream E comprising at least one hydrocarbon and at least one aminating reagent to form a reaction mixture R comprising aminohydrocarbons and hydrogen and b) electrochemical separation of at least part of the hydrogen formed in the reaction from the reaction mixture R by means of a gastight membrane-electrode assembly having at least one selectively proton-conducting membrane and at least one electrode catalyst on each side of the membrane, where at least part of the hydrogen is oxidized to protons over the anode catalyst on the retentate side of the membrane and the protons are, after passing through the membrane, b1) reduced to hydrogen and/or b2) reacted with oxygen from an oxygen-comprising stream O which is brought into contact with the permeate side of the membrane to form water over the cathode catalyst on the permeate side.

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10-05-2012 дата публикации

Process for separating one or more aliphatic diamines from reductive amination reaction solvents and impurities

Номер: US20120116123A1
Принадлежит: Dow Global Technologies LLC

The instant invention provides a process for separating one or more aliphatic diamines from reductive amination reaction solvents and impurities, and aliphatic diamines obtained via such a process. The process for separating one or more aliphatic diamines from reductive amination reaction solvents and impurities according to the instant invention comprises the steps of: (1) feeding one or more cycloaliphatic cyanoaldehydes, hydrogen, ammonia, and optionally one or more solvents into a continuous reductive amination reactor system; (2) contacting said one or more cycloaliphatic cyanoaldehydes, hydrogen, and ammonia with each other in the presence of one or more heterogeneous metal based catalyst systems at a temperature in the range of from 80° C. to about 160° C. and a pressure in the range of from 700 to 3500 psig; (3) thereby forming a product mixture comprising one or more cycloaliphatic diamines, optionally one or more bicyclic by-products, optionally one or more cycloaliphatic aminonitriles, optionally one or more cycloaliphatic aminoalcohols, optionally one or more oligomeric by-products, ammonia, water, hydrogen, and optionally one or more solvents; (4) removing said product mixture from the reactor system; (5) removing at least a portion of said ammonia, said hydrogen, or mixture thereof from said product mixture via distillation; (6) removing at least a portion of said water and said one or more optional solvents via distillation; (7) removing at least a portion of one or more optional bicyclic by-products via distillation; (8) removing one or more optional cycloaliphatic aminonitriles, one or more optional cycloaliphatic aminoalcohols, one or more optional oligomeric by-products via distillation; and (9) thereby separating said one or more cycloaliphatic diamines from said product mixture.

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24-05-2012 дата публикации

Method of preparing 1-chloroacetamido-1,3,3,5,5-pentamethylcyclohexane

Номер: US20120130127A1
Принадлежит: Mer Pharma GmbH and Co KGaA

Method of preparing 1-chloroacetamido-1,3,3,5,5-pentamethylcyclohexane, an intermediate in the synthesis of 1-amino-1,3,3,5,5-pentamethylcyclohexane (Neramexane) or a pharmaceutically acceptable salt thereof, comprising step (iii): (iii) reacting 1-hydroxy-1,3,3,5,5-pentamethylcyclohexane with chloroacetonitrile in the presence of an acid, wherein 1-hydroxy-1,3,3,5,5-pentamethylcyclohexane is employed in step (iii) as obtained in the reaction of a methylmagnesium halide with 3,3,5,5-tetramethylcyclohexanone without having been subjected to a purification step.

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31-05-2012 дата публикации

Process for improving the catalytic activity of catalyst systems for reductive amination of aliphatic cyanoaldehydes to aliphatic diamines

Номер: US20120136173A1
Принадлежит: Dow Global Technologies LLC

The instant invention provides a process for improving catalytic activity of catalyst systems for reductive amination of aliphatic cyanoaldehydes to aliphatic diamines. The process for improving catalytic activity of catalyst systems for reductive amination of aliphatic cyanoaldehydes to aliphatic diamines comprises the steps of: (1) feeding ammonia, optionally hydrogen, and optionally one or more solvents over one or more heterogeneous metal based catalyst systems having a reduced catalytic activity for a period of greater than 1 hour at a temperature in the range of from 50° C. to 500° C.; wherein said one or more heterogeneous metal based catalyst systems have a yield of less than 90 percent based on the molar conversion of cyanoaldehydes to diamines; and (2) thereby improving the catalytic activity of said one or more heterogeneous metal based catalyst systems.

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28-06-2012 дата публикации

Novel compound and method for preparing the same

Номер: US20120165572A1
Принадлежит: Fujifilm Corp

The invention is directed to a compound represented by the Formula (1) as defined herein, and a method for preparing a compound represented by the Formula (1) which includes: reacting a diamine compound represented by the Formula (2) as defined herein with a methacrylic anhydride or an acrylic anhydride under a condition where an organic acid having a pKa of 2.0 or more is present in an amount of 0.5 to 5.0 moles based on 1 mole of the diamine compound to obtain a reaction mixture; adding phosphoric acid to the reaction mixture; and purifying the reaction mixture by extraction with an organic solvent.

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05-07-2012 дата публикации

Continuous method for the hydrogenation of aromatic compounds

Номер: US20120172632A1
Принадлежит: AET Group

The invention relates to a continuous method for the catalytic hydrogenation of an aromatic compound into a cycloaliphatic compound, wherein said method is carried out in a piston reactor provided with a mechanical axially agitating means and comprises continuously feeding a liquid phase comprising said aromatic compound and a catalyst dispersed to the liquid phase, subjecting said liquid phase, at a temperature of between 100° C. and 300° C. and while being mechanical axially agitated, to the effects of a hydrogen pressure of between 10 and 250 bars in the presence of said catalyst dispersed in the liquid phase for a residence time of between 1 second and 10 minutes, and removing the liquid phase from the reactor.

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26-07-2012 дата публикации

Hydrochlorination of electron-deficient alkenes

Номер: US20120190879A1
Автор: Michael Todd Coleman
Принадлежит: Future Fuel Chemical Co

The present invention pertains to a method for the hydrochlorination of electron deficient alkenes, particularly alkenes having the functional groups COOH, CONH 2 , and CN. Specific alkenes discussed include acrylic acid, crotonic acid, methacrylic acid, acrylonitrile, acrylamide, and methacrylonitrile. The alkene is combined with a primary or secondary alcohol (e.g., isopropanol) and an acid chloride (e.g., acetyl chloride) under conditions suitable to chlorinate the alkene. Products formed by the invention include 3-chorosubstituted carbonyl compounds such as 3-chlorpropionic acid (3-CPA), 3-chloropropionamide (3-CPAD), and 3-chloropropionitrile among other products.

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27-09-2012 дата публикации

Process for hydrogenating nitriles

Номер: US20120245390A1
Принадлежит: BASF SE

The present invention relates to a process for hydrogenating nitriles by means of hydrogen in the presence of a catalyst in a reactor, where the catalyst is arranged in a fixed bed, wherein the cross-sectional loading in the reactor is in the range from 5 kg/(m 2 s) to 50 kg/(m 2 s). The present invention further relates to a process for preparing downstream products of isophoronediamine (IPDA) or N,N-dimethylaminopropylamine (DMAPA) from amines prepared according to the invention.

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22-11-2012 дата публикации

Catalyst and process for hydrogenating aromatics

Номер: US20120296111A1
Принадлежит: BASF SE

The present invention relates to an eggshell catalyst comprising an active metal selected from the group consisting of ruthenium, rhodium, palladium, platinum and mixtures thereof, applied to a support material comprising silicon dioxide, wherein the pore volume of the support material is 0.6 to 1.0 ml/g, determined by Hg porosimetry, the BET surface area is 280 to 500 m 2 /g, and at least 90% of the pores present have a diameter of 6 to 12 nm, to a process for preparing this eggshell catalyst, to a process for hydrogenating an organic compound which comprises at least one hydrogenatable group using the eggshell catalyst, and to the use of the eggshell catalyst for hydrogenating an organic compound.

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03-01-2013 дата публикации

Process for the conversion of aromatic nitro compound into amines

Номер: US20130006018A1
Принадлежит: Huntsman International LLC

A process for hydrogenating an aromatic nitro compound according to the invention comprises providing a hydrogen gas stream and a liquid aromatic nitro compound stream; providing a fixed bed catalytic reactor having an inflow side and an outflow side; feeding to the inflow side, the hydrogen gas stream and the liquid aromatic nitro compound stream; converting the hydrogen gas and the aromatic nitro compound into an aromatic amine, thereby providing a reactor effluent comprising the aromatic amine and water; evacuating the reactor effluent from the reactor at the outflow side of the reactor; wherein an inert solvent or water is fed to the inflow side of the reactor at a molar ratio of moles inert solvent or water to moles hydrogen is more than 1.

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21-02-2013 дата публикации

Method for the Hydrolysis of Substituted Formylamines into Substituted Amines

Номер: US20130046111A1
Автор: Mikhail Bobylev
Принадлежит: Individual

An improved method for the synthesis of substituted formylamines and substituted amines via an accelerated Leuckart reaction. The Leuckart reaction is accelerated by reacting formamide or N-alkylformamide and formic acid with an aldehyde or a ketone at a preferred molar ratio that accelerates the reaction. The improved method is applicable to various substituted aldehydes and ketones, including substituted benzaldehydes. An accelerated method for the hydrolysis of substituted formylamines into substituted amines using acid or base and a solvent at an elevated temperature. The improved method is useful for the accelerated synthesis of agrochemicals and pharmaceuticals such as vanillylamine, amphetamine and its analogs, and formamide fungicides.

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28-02-2013 дата публикации

Process for preparing eddn and/or edmn and a process for preparing deta and/or teta

Номер: US20130053536A1
Принадлежит: BASF SE

A process for preparing EDDN and/or EDMN by a) conversion of FA, HCN and EDA, the conversion being effected in the presence of water, b) depleting water from the reaction mixture obtained in stage a), and c) treating the mixture from stage b) with an absorbent in the presence of an organic solvent, wherein the adsorbent is a solid acidic adsorbent.

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21-03-2013 дата публикации

18ß-GLYCYRRHETINIC ACID DERIVATIVES AND SYNTHETIC METHOD THEREOF

Номер: US20130072694A1
Принадлежит: KAOHSIUNG MEDICAL UNIVERSITY

The present invention provides a chemical compound having the structure being one selected from a group consisting of 2. The method according to further comprising a step of using an isopropylamine solution as the amine solution when Ris CONHCH(CH) claim 1 , and using an aniline solution as the amine solution when Ris CONHCH.3. The method according to further comprising steps of:methylating the 18β-glycyrrhetinic acid to obtain a methylated 18β-glycyrrhetinic acid; andoxidizing the methylated 18β-glycyrrhetinic acid to obtain a second compound.4. The method according to further comprising a step of esterifying the lactone compound to obtain a first derivative of the lactone compound.5. The method according to further comprising a step of cleaving a lactone ring of the lactone compound to obtain a second derivative of the lactone compound.6. The method according to further comprising a step of treating the second derivative with an alcohol solution to obtain a third derivative of the lactone compound.7. The method according to claim 6 , wherein the alcohol solution is one of an isopropyl alcohol solution and a benzyl alcohol solution.8. The method according to further comprising a step of esterifying the second compound with an alcohol solution to obtain a fourth derivative of the lactone compound.9. The method according to further comprising a step of cleaving a lactone ring of the fourth derivative by an acidic solution to obtain a fifth derivative of the lactone compound.13. The method according to claim 12 , wherein the chemical compound with Rbeing one of CONHCH(CH)and CONHCHis obtained by steps of:oxidizing the 18β-glycyrrhetinic acid to form a first compound;treating the first compound with an m-chloroperbenzoic acid to afford a lactone compound; andtreating the lactone compound with an amine solution to obtain the chemical compound being a first derivative of the chemical compound.14. The method according to further comprising a step of using an ...

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21-03-2013 дата публикации

Supported metal catalysts

Номер: US20130072722A1
Принадлежит: JOHNSON MATTHEY PLC

The present invention relates to supported metal catalysts, wherein the catalysts are modified by at least one amine, a method for the preparation thereof and hydrogenation processes utilising the supported metal catalysts.

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28-03-2013 дата публикации

Process for preparing eddn and edmn

Номер: US20130079492A1
Принадлежит: BASF SE

A process for preparing EDDN and/or EDMN by conversion of FA, HCN and EDA, the reaction being effected in the presence of water, and, after the conversion, water being depleted from the reaction mixture in a distillation column, which comprises performing the distillation in the presence of an organic solvent which has a boiling point between water and EDDN and/or EDMN at the distillation pressure existing in the column or which forms a low-boiling azeotrope with water.

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28-03-2013 дата публикации

METHOD FOR PRODUCING beta-AMINOCARBONYL COMPOUND

Номер: US20130079543A1

An optically active β-aminocarbonyl compound is obtained by a Mannich reaction between an aldimine in which: nitrogen is protected and a malonic acid diester, in the presence of optically active BINOL and dialkyl magnesium (in which two alkyl groups are the same or different) in an amount 1 to 2 molar times the amount of the BINOL. 1. A method for producing a β-aminocarbonyl compound comprising carrying out a Mannich reaction between an aldimine in which nitrogen is protected and a malonic acid diester , in the presence of optically active BINOL and dialkyl magnesium (in which two alkyl groups are the same or different) in an amount 1 to 2 molar times the amount of the BINOL , to obtain an optically active β-aminocarbonyl compound.2. The method for producing a β-aminocarbonyl compound according to claim 1 , wherein the aldimine is a compound represented by R—CH═NR(wherein Ris an aryl group or an ester group claim 1 , and Ris tert-butoxycarbonyl (Boc) claim 1 , benzyloxycarbonyl (Cbz) claim 1 , 2 claim 1 ,2 claim 1 ,2-trichloroethoxycarbonyl (Troc) claim 1 , a phenyl group claim 1 , a 2-methoxyphenyl group claim 1 , a 4-methoxyphenyl group claim 1 , or a naphthyl group).3. The method for producing a β-aminocarbonyl compound according to claim 1 , wherein the malonic acid diester is a compound represented by CHX(COR)(wherein X is a hydrogen atom or a halogen atom claim 1 , and Ris alkyl claim 1 , allyl claim 1 , benzyl claim 1 , or aryl).4. The method for producing a β-aminocarbonyl compound according to claim 1 , wherein the BINOL is used in an amount of 2.5 mole percent to 10 mole percent relative to the aldimine.5. The method for producing a β-aminocarbonyl compound according to claim 1 , wherein an aromatic solvent or a halogenated hydrocarbon solvent is used as a reaction solvent. The present invention relates to a method for producing a β-aminocarbonyl compound.Mannich reactions in which a carbonyl compound is added directly to an aldimine are one. Of the most ...

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28-03-2013 дата публикации

METHOD FOR PREPARING ALKYL LACTATE AND A METHOD FOR PREPARING LACTAMIDE USING THE SAME

Номер: US20130079547A1
Принадлежит: LG CHEM, LTD.

This disclosure relates to a method for preparing alkyl lactate with high yield and high selectivity, comprising the step of reacting glycerol with water or alcohol in the presence of a catalyst. 2. The method according to claim 1 , wherein the catalyst is a homogeneous or heterogeneous catalyst.3. The method according to claim 2 , wherein the homogeneous catalyst is at least one selected from the group consisting of an alkali metal compound having a hydroxyl or alkoxy group claim 2 , a bicarbonate (HCO)-containing metal compound claim 2 , and a carbonate (CO)-containing metal compound.4. The method according to claim 3 , wherein the alkali metal compound having a hydroxyl group is NaOH claim 3 , KOH claim 3 , LiOH or Ba(OH) claim 3 , andthe alkali metal compound having an alkoxy group is NaOR, KOR or LiOR (wherein, R is a substituted or unsubstituted C1-10 alkyl group).5. The method according to claim 2 , wherein the heterogeneous catalyst is a metal compound containing Mg claim 2 , Ca claim 2 , Zr claim 2 , Sn or Ti.6. The method according to claim 5 , wherein the heterogeneous catalyst further comprises at least one selected from the group consisting of an alkali metal compound claim 5 , a hydroxyl group-containing metal compound claim 5 , a bicarbonate-containing metal compound claim 5 , a carbonate-containing metal compound claim 5 , activated clay claim 5 , zeolite claim 5 , active carbon claim 5 , diatomaceous earth claim 5 , bentonite claim 5 , alumina claim 5 , silicalite claim 5 , fly ashes claim 5 , molecular sieve claim 5 , vermiculite claim 5 , perlite claim 5 , π-complex compound adsorbent claim 5 , clay and polymer resin.7. The method according to claim 1 , wherein the reaction is conducted in a batch reactor or tubular reactor.8. The method according to claim 1 , wherein the reaction is conducted at a temperature of 100 to 300° C. and a pressure of 10 to 200 atm for 1 to 20 hours claim 1 , under inert atmosphere.9. The method according to claim 1 , ...

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28-03-2013 дата публикации

SOLID BASE CATALYST AND METHOD FOR MAKING AND USING THE SAME

Номер: US20130079560A1
Автор: CHEN Xinmin, Zhu Jianliang
Принадлежит: Jiangsu Sinorgchem Technology Co., Ltd.

A solid base catalyst having a carrier, an organic base, and an inorganic base. Both of the organic base and inorganic base are loaded on the carrier. The solid base catalyst is especially suitable for the synthesis of 4-Aminodiphenylamine (4-ADPA). 1. A solid base catalyst comprisingan organic base,an inorganic base; anda carrier,wherein the organic base is chemically bound to the carrier, and the inorganic base is adsorbed in the carrier.2. The solid base catalyst of claim 1 , wherein the organic base is methylamine claim 1 , ethylamine claim 1 , cyclohexylamine claim 1 , aniline claim 1 , phenyl diamine claim 1 , dodecyl trimethyl ammonium chloride claim 1 , trimethyl benzyl ammonium chloride claim 1 , tetramethyl ammonium chloride claim 1 , tetramethyl ammonium bromide claim 1 , tetramethyl ammonium hydroxide claim 1 , tetraethyl ammonium hydroxide claim 1 , tetrapropyl ammonium hydroxide claim 1 , tetrabutyl ammonium hydroxide claim 1 , tetramethyl ammonium hydroxide claim 1 , benzyl trimethyl ammonium hydroxide claim 1 , benzyl triethyl ammonium hydroxide claim 1 , 4-dimethylamino pyridine claim 1 , crown ether claim 1 , or a mixture thereof.3. The solid base catalyst of claim 1 , wherein the organic base is tetramethyl ammonium hydroxide or tetraethyl ammonium hydroxide.4. The solid base catalyst of wherein the inorganic base is potassium hydroxide claim 1 , sodium hydroxide claim 1 , calcium hydroxide claim 1 , cesium hydroxide claim 1 , aluminum hydroxide claim 1 , sodium methoxide claim 1 , sodium ethoxide claim 1 , potassium methoxide claim 1 , potassium ethoxide claim 1 , or a mixture thereof.5. The solid base catalyst of claim 1 , wherein the inorganic base is potassium hydroxide or sodium hydroxide.6. The solid base catalyst of claim 1 , wherein the carrier is alumina claim 1 , silica gel claim 1 , diatomite claim 1 , molecular sieve claim 1 , macroporous adsorption resin claim 1 , or a mixture thereof.7. The solid base catalyst of claim 6 , wherein ...

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04-04-2013 дата публикации

Unknown

Номер: US20130085286A1
Принадлежит: BASF SE

A process for preparing amines of the formula (II) 111-. (canceled)13. The process of claim 12 , wherein the nitriles are ethylenediaminediacetonitrile claim 12 , ethylenediaminemonoacetonitrile claim 12 , or iminodiacetonitrile.14. The process of claim 12 , wherein the hydrogenation is effected at a temperature in the range from 60 to 150° C.15. The process of claim 13 , wherein the hydrogenation is effected at a temperature in the range from 60 to 150° C.16. The process of claim 12 , wherein the pressure existing in the hydrogenation is in the range from 170 to 240 bar.17. The process of claim 15 , wherein the pressure existing in the hydrogenation is in the range from 170 to 240 bar.18. The process of claim 12 , wherein the hydrogenation is effected in the presence of an organic solvent.19. The process of claim 17 , wherein the hydrogenation is effected in the presence of an organic solvent.20. The process of claim 12 , wherein the hydrogenation is effected in the presence of tetrhydrofuran.21. The process of claim 12 , wherein the hydrogenation is effected in the presence of tetrahydrofuran and toluene.22. The process of claim 19 , wherein the hydrogenation is effected in the presence of tetrhydrofuran.23. The process of claim 19 , wherein the hydrogenation is effected in the presence of tetrahydrofuran and toluene.24. The process of claim 12 , wherein the nitrile of formula (I) is treated before the hydrogenation with an adsorbent in the presence of an organic solvent.25. The process of claim 24 , wherein the adsorbent is a solid acidic adsorbent.26. The process of claim 12 , wherein the space velocity is 0.25·10to 5·10kg of nitrile of formula (I) per mof catalyst surface area and hour.27. A process for preparing an epoxy resin claim 12 , amide claim 12 , or polyamide claim 12 , which comprises in a first stage preparing triethylenetetramine or diethylenetriamine by the process of claim 12 , and in a second stage converting the triethylenetetramine or ...

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11-04-2013 дата публикации

PROCESS FOR PREPARING EDDN AND/OR EDMN BY CONVERSION OF FACH AND EDA

Номер: US20130090452A1
Принадлежит: BASF SE

A process for reacting formaldehyde cyanohydrin (FACH) with ethylenediamine (EDA) in a reactor with limited backmixing at a temperature in the range from 20 to 120° C., wherein the residence time in the reactor is 300 seconds or less. 116-. (canceled)17. A process for reacting formaldehyde cyanohydrin (FACH) with ethylenediamine (EDA) in a reactor with limited backmixing at a temperature in the range from 20 to 120° C. , wherein the residence time in the reactor is 300 seconds or less.18. The process according to claim 17 , wherein the residence time in the reactor is less than 60 seconds.19. The process according to claim 17 , wherein the reactor is a tubular reactor.20. The process according to claim 17 , wherein the inlet temperature of the reactants into the reactor is in the range from 10 to 50° C.21. The process according to claim 17 , wherein the reaction is effected in the presence of one or more organic solvents.22. The process according to claim 17 , wherein the conversion is performed in the presence of water.23. The process according to claim 22 , wherein at least a portion of the water is mixed with EDA before entry into the reactor and the resulting mixture is then cooled.24. The process according to claim 17 , wherein the reaction mixture is cooled after it leaves the reactor.25. The process according to claim 17 , wherein the reaction mixture is cooled by flash evaporation.26. The process according to claim 25 , wherein the pressure in the flash evaporation step is less than 300 mbar.27. The process according to at least one of claim 21 , wherein the organic solvent has a miscibility gap with water.28. The process according to claim 27 , wherein the organic solvent which has a miscibility gap with water is toluene.29. The process according to at least one of claim 17 , wherein the tubular reactor is additionally cooled by means of a cooling jacket.Ethylenediamine (EDA)Ethylenediamine-formaldehyde bisadduct (EDFA)Ethylenediamine-formaldehyde ...

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11-04-2013 дата публикации

Process for preparing TETA and DETA

Номер: US20130090453A1
Принадлежит: BASF SE

A process for preparing TETA and/or DETA by hydrogenating EDDN and/or EDMN with hydrogen in the presence of a catalyst, which comprises preparing EDDN and/or EDMN from FA, HCN and EDA in the presence of toluene as a solvent and performing the hydrogenation in suspension mode in the presence of THF. 16-. (canceled)7. A process for preparing triethylenetetramine (TETA) and/or diethylenetriamine (DETA) by hydrogenating ethylenediaminediacetonitrile (EDDN) and/or Ethylenediaminemonoacetonitrile (EDMN) with hydrogen in the presence of a catalyst , which comprises preparing EDDN and/or EDMN from formaldehyde (FA) , hydrogen cyanide (HCN) and ethylenediamine (EDA) in the presence of toluene as a solvent and performing the hydrogenation in suspension mode in the presence of tetrahydrofuran.8. The process of claim 7 , wherein HCN and EDA are first converted to formaldehyde cyanohydrin claim 7 , which is subsequently reacted with EDA.9. The process of claim 7 , wherein EDDN is obtained by reacting an ethylenediamine-formaldehyde adduct (EDFA) claim 7 , or EDMN by reacting an ethylenediamine-monoformaldehyde adduct (EDMFA) claim 7 , with HCN claim 7 , EDFA or EDMFA being obtained by reacting EDA with FA.10. The process of claim 7 , wherein the output from the EDDN or EDMN preparation is treated with a solid acidic adsorbent in the presence of tetrahydrofuran.11. The process of claim 7 , wherein the reaction output from the hydrogenation which is obtained in the reaction of EDDN or EDMN with hydrogen in the presence of tetrahydrofuran and a catalyst and which comprises TETA or DETA and water claim 7 , with or without organic compounds having higher and lower boiling points than TETA or DETA claim 7 , is separated claim 7 , wherein{'b': '1', 'i) the reaction output after removal of hydrogen is supplied to a distillation column DK in which a tetrahydrofuran/water azeotrope is removed via the top and which may also comprise further organic compounds having a lower boiling point ...

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11-04-2013 дата публикации

GOLD COMPLEXES FOR USE IN THE TREATMENT OF CANCER

Номер: US20130090472A1
Принадлежит: UNIVERSITY OF KWAZULU-NATAL

The invention provides compounds of the Formula (I), in which W is independently selected from W, W, W, W, W, or W represents a pair of substituents independently selected from H, alkyl, aryl or amide in which the amide is optionally part of a linking chain, and the Z—Zbonds (n=4-17; n′=n+1) are optionally of any whole or partial bond order, Y is Yor Y represents a pair of substituents independently selected from H, C--Calkyl, Zor Zaryl, or Y is optionally a bridging structure that may comprise one or more C--Camide, C--Cether, or C--Cester groups, R-Rare independently selected from no substituent, a lone pair of electrons, H, halogen, C-Caryl, C- C-alkyl, amine, C--Calkylamine, C--Camide, nitro, cyano, carboxyl, C--Cester, phosphane, thiol, C--Cthioether, OR′, and suitable pairs of adjacent R groups (R-R) may optionally together form part of a Cor Caryl ring, a Zor Zring, R′ is independently selected from H, C--Calkyl, Zor Zaryl, C--Cester, poly(—CO—), amine, and C--Calkylamine, Z-Zare independently selected from C, N, P, O, and S, and X is a pharmaceutically acceptable anion, for the treatment of cancer. 2. The compound of claim 1 , in which the anion is selected from halide claim 1 , hexafluorophosphate claim 1 , nitrate claim 1 , and triflate.3. The compound of claim 1 , in which Y represents two hydrogen atoms or Y.4. The compound of claim 3 , in which Y is Yand Zand Zare N.5. The compound of claim 4 , in which Z-Zare C.6. The compound of claim 1 , in which R-Rare selected from H claim 1 , C-Calkyl claim 1 , O—C-Calkyl claim 1 , hydroxyl and halogen.7. The compound of claim 6 , in which C-Calkyl is methyl claim 6 , O—C-Calkyl is O-ethyl claim 6 , and halogen is chlorine.8. The compound of claim 1 , in which W is selected from W claim 1 , W claim 1 , WWor W.9. The compound of claim 8 , in which R-Rare selected from H claim 8 , C-Calkyl claim 8 , O—C-Calkyl and halogen.10. The compound of claim 9 , in which C-Calkyl is methyl claim 9 , O—C-Calkyl is O-ethyl and ...

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18-04-2013 дата публикации

SYNTHESIS OF AZO BONDED IMMUNOREGULATORY COMPOUNDS

Номер: US20130096286A1
Принадлежит:

Methods are disclosed for preparing compounds of Formula I: 3. The method of claim 1 , wherein the nitrile or amide is hydrolyzed to the carboxylic acid using acid catalysis.4. The method of claim 1 , wherein the nitrile or amide is hydrolyzed to the carboxylic acid using basic catalysis.5. The method of claim 1 , wherein the nitrile or amide is hydrolyzed to the carboxylic acid using enzymatic catalysis.6. The method of claim 1 , wherein the isolation step involves enzymatic resolution of one of the enantiomers during the hydrolysis of a nitrile or amide group.7. The method of claim 1 , wherein R claim 1 , R claim 1 , and Rare independently selected from the group consisting of H claim 1 , CH claim 1 , CHCH claim 1 , and CH(CH).8. The method of claim 1 , wherein R claim 1 , R claim 1 , and Rare independently selected from the group consisting of H claim 1 , CH claim 1 , CHCH claim 1 , and CH(CH).9. The method of claim 1 , wherein Ris selected from the group consisting of H claim 1 , CH claim 1 , CHCH claim 1 , and CH(CH).10. The method of claim 1 , wherein the compound that is formed is 5-(4-carboxymethyl-phenylazo)-2-hydroxy-benzoic acid claim 1 , 5-[4-(1-carboxy-ethyl)-phenylazo]-2-hydroxy-benzoic acid or 4-(4-carboxymethyl-phenylazo)-phenylacetic acid. This application is a divisional application of U.S. patent application Ser. No. 13/094,135 filed on Apr. 26, 2011, now U.S. Pat. No. 8,314,214 which in turn was a divisional application of Ser. No. 11/631,582, filed on Jan. 4, 2007, now U.S. Pat. No. 7,932,366, which in turn was filed under the provisions of 35 U.S.C. §371 and claimed priority of International Patent Application No. PCT/US2005/024109, filed on Jul. 7, 2005, and which in turn claimed priority of U.S. Provisional Application No. 60/585,995 filed on Jul. 7, 2004.1. Field of the InventionThe present invention relates to immunoregulatory compounds, methods of producing same and methods of treating diseases therewith.2. Background of the InventionMany ...

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18-04-2013 дата публикации

RESOLUTION METHODS FOR ISOLATING DESIRED ENANTIOMERS OF TAPENTADOL INTERMEDIATES AND USE THEREOF FOR THE PREPARATION OF TAPENTADOL

Номер: US20130096346A1
Принадлежит: ACTAVIS GROUP PTC EHF

Provided herein is an improved and industrially advantageous optical resolution method for resolving (2R,3R)/(2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol, and use thereof for the preparation of tapentadol or a pharmaceutically acceptable salt thereof. Provided further herein is an improved and industrially advantageous optical resolution method for resolving (2R,3R)/(2S,3S)-[3-(3-methoxyphenyl)-2-methylpentyl]-dimethylamine, and use thereof for the preparation of tapentadol or a pharmaceutically acceptable salt thereof. Disclosed also herein is an improved, commercially viable and industrially advantageous process for the preparation of tapentadol or a pharmaceutically acceptable salt thereof in high yield and purity. 2. The process of claim 1 , wherein the first solvent used in step-(a) is selected from the group consisting of water claim 1 , an alcohol claim 1 , a ketone claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a nitrile claim 1 , an ester claim 1 , a polar aprotic solvent claim 1 , and mixtures thereof; wherein the second solvent used in step-(c) is selected from the group consisting of water claim 1 , an alcohol claim 1 , a ketone claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a nitrile claim 1 , an ester claim 1 , and mixtures thereof; and wherein the base used in step-(c) is selected from the group consisting of triethylamine claim 1 , trimethylamine claim 1 , dimethyl amine claim 1 , tert-butyl amine claim 1 , aqueous ammonia claim 1 , sodium hydroxide claim 1 , calcium hydroxide claim 1 , magnesium hydroxide claim 1 , potassium hydroxide claim 1 , lithium hydroxide claim 1 , sodium carbonate claim 1 , potassium carbonate claim 1 , sodium bicarbonate claim 1 , potassium bicarbonate claim 1 , lithium carbonate claim 1 , sodium tert-butoxide claim 1 , sodium isopropoxide and potassium ...

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18-04-2013 дата публикации

Process for conversion of isobutylene to tertiary butylamine

Номер: US20130096349A1
Принадлежит: Individual

The invention discloses an improved process for the conversion of isobutylene to tertiary butylamine with conversion up to 50% at pressure lower than 40 bar.

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18-04-2013 дата публикации

Method to Recover Organic Tertiary Amines from Waste Sulfuric Acid

Номер: US20130096350A1

The present invention describes a method to recover organic tertiary amines from waste sulfuric acid comprising the following steps: 1. Method to recover organic tertiary amines from waste sulfuric acid comprising the following steps: 'ii) ammonia in an amount sufficient to obtain a pH of 9.5 or higher and', 'a) reacting i) waste sulfuric acid comprising organic tertiary amines with'}b) separating the organic tertiary amines from the reaction mixture obtained in step a) wherein during the separation the pH of the reaction mixture is adjusted to a pH of 9.5 or higher.2. Method according to wherein the organic tertiary amine is separated from the reaction mixture obtained in step a) in a distillation column.3. Method according to wherein during the distillation ammonia is added to the distillation column.4. Method according to wherein during the distillation ammonia is added to the distillation column in a counter flow to the reaction mixture obtained in step a).5. Method according to wherein during the distillation the reaction mixture obtained in step a) is continuously fed to the upper part of a distillation column and the ammonia is continuously fed to the lower part or the middle part of the distillation column.6. Method according to wherein the ammonia feed to the distillation column is positioned such that the aqueous solution which is essentially free of organic tertiary amine and which comprises the ammonium sulfate in the lower part of the column has a pH ranging from 5 to 7.7. Method according to wherein the organic tertiary amine is separated fro the reaction mixture by extraction with an organic liquid claim 1 , preferably a liquid hydrocarbon claim 1 , more preferably an aliphatic liquid hydrocarbon comprising at least 6 carbon atoms claim 1 , especially octane.8. Method according to wherein the pH in step a) and/or step b) ranges from 9.8 to 12.9. Method according to wherein the organic tertiary amine is triethylamine.10. Method according to wherein the ...

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25-04-2013 дата публикации

PROCESS FOR THE PREPARATION OF LACOSAMIDE

Номер: US20130102811A1
Принадлежит: SUN PHARMACEUTICAL INDUSTRIES LTD

The present invention relates to a novel and improved process for the preparation of lacosamide, wherein the process is a sequential one-pot process. 2. The process as claimed in claim 1 , wherein all the reactions of step a) to d) are carried out in dicholormethane.3. The process as claimed in claim 1 , wherein the condensation of N-Boc-D-serine with benzylamine in step a) is performed using a coupling agent claim 1 , optionally in the presence of catalytic 1-hydroxybenzitriazole4. The process as claimed in claim 3 , wherein the coupling agent is selected from the group consisting of (benzotriazole- 1-yloxy)tris(dimethylamino)phosphonium hexafluorophosphate (BOP) claim 3 , is obutyl chloroformate claim 3 , N claim 3 ,N′-dicyclohexylcarbodiimide (DCC) and N-(3-dimethylaminopropyl)-N-ethylcarbodiimide(EDC).5. The process as claimed in claim 1 , wherein methylation of compound of formula I in step b) is carried out using a methylating agent in a biphasic system in presence of a phase transfer catalyst.6. The process as claimed in claim 5 , wherein the methylating agent is selected from the group consisting of dimethyl sulfate claim 5 , methyl triflate claim 5 , and trimethyl phosphate.7. The process as claimed in claim 6 , wherein the methylating agent is dimethyl sulfate.8. The process as claimed in claim 5 , wherein the aqueous phase of the biphasic system contains an inorganic base.9. The process as claimed in claim 8 , wherein the inorganic base is selected from an alkali metal hydroxide claim 8 , carbonate and bicarbonate.10. The process as claimed in claim 5 , wherein the phase transfer catalyst is selected from a quarternized amine salt or a phosphonium salt.11. The process as claimed in claim 10 , wherein quarternized amine salt is selected from the group consisting of sulfate claim 10 , chloride or bromide salts of tetraalkylammonium; benzyltrialkylammonium halides; cetyltrialkylammonium halides and Tweens (polyoxyethylene sorbitan esters) such as Tween®20 ...

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02-05-2013 дата публикации

PHENYL-N-ACYL DERIVATIVES OF AMINES AND AMINO ACIDS, A PROCESS FOR THE PREPARATION THEREOF, A PHARMACEUTICAL COMPOSITION AND USE THEREOF

Номер: US20130109880A1

The present invention relates to novel phenyl-N-acyl derivatives of biogenic amines and amino acids of general formula (I) as cyclooxynease inhibitors, possessing analgetic and anti-inflammatory properties and devoid of side effects in particular ulcerogeneity and pro-spasmodic actions, as well as capability to potentiate effect of other analgetics, and possessing in addition antihypoxic, antidepressant and anti-Parkinsonistic action; as well as to the processes for the preparation novel and known phenyl-N-acyl derivatives of biogenic amines, to a pharmaceutical composition and to an agent comprising compounds of general formula (I) as well as to use thereof and a method of treating. 2. The process according to claim 1 , wherein 1-1.2 equivalents of diphenylphosphorylazide and triethylamine are used.3. The process according to claim 1 , wherein as amino derivatives tyrosine or phenylalanine esters are used.43. The process according to any one of - claims 1 , wherein as an organic solvent N claims 1 ,N-dimethylformamide or ethylacetate are used.53. The process according to any one of - claims 1 , which is conducted at the temperature ranging from −25° C. to 0° C.7. The process according to claim 6 , wherein as amino derivatives tyrosine or phenylalanine esters are used. This application is a divisional of co-pending U.S. application Ser. No. 11/886,965, filed on Oct. 23, 2008, which is a U.S. National Stage application under 35 U.S.C. §371 of International Application PCT/RU2006/000139 (published as WO 2006/101422 A1), filed Mar. 24, 2006, which claims priority to Application RU 2005108492, filed Mar. 25, 2005. Benefit of the filing date of each of these prior applications is hereby claimed. Each of these prior applications is hereby incorporated by reference in its entirety.The present invention relates to the field of bioorganic chemistry and concerns novel compounds, phenyl-N-acyl derivatives of biogenic amines as well as a process for synthesis of novel and known ...

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16-05-2013 дата публикации

METHOD FOR SYNTHESIZING RARE EARTH METAL EXTRACTANT

Номер: US20130123534A1
Принадлежит:

A rare earth metal extractant containing, as the extractant component, dialkyldiglycol amide acid which is excellent in breaking down light rare earth elements is reacted in diglycolic acid (X mol) and an esterification agent (Y mol) at a reaction temperature of 70° C. or more and for a reaction time of one hour or more such that the mol ratio of Y/X is 2.5 or more, and is subjected to vacuum concentration. Subsequently, a reaction intermediate product is obtained by removing unreacted products and reaction residue. Then a nonpolar or low-polar solvent which is an organic solvent for forming an organic phase during solvent extraction of the rare earth metal and which is capable of dissolving dialkyldiglycol amide acid is added as the reaction solvent, and the reaction intermediate product is reacted with dialkyl amine (Z mol) such that the mol ratio of Z/X is 0.9 or more. 2. A method for synthesizing a rare earth metal extractant according to wherein the esterifying agent is selected from acetic anhydride and trifluoroacetic anhydride.3. A method for synthesizing a rare earth metal extractant according to wherein the organic solvent to form an organic phase during solvent extraction of rare earth metals is selected from the group consisting of toluene claim 1 , xylene claim 1 , hexane claim 1 , isododecane claim 1 , kerosene claim 1 , and higher alcohols.4. A method for synthesizing a rare earth metal extractant according to wherein in the step of reacting diglycolic acid with an esterifying agent claim 1 , the molar ratio of Y/X is in the range: 2.5≦Y/X≦6.5.5. A method for synthesizing a rare earth metal extractant wherein in the step of reacting the reaction intermediate product with a dialkylamine claim 1 , the molar ratio of Z/X is in the range: 0.9≦Z/X≦1.2.6. A method for synthesizing a rare earth metal extractant wherein the reaction solvent is added in such an amount that the dialkyl diglycol amic acid formed after the reactions may be present in a ...

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16-05-2013 дата публикации

LIQUID PHENOL RESIN AND METHOD OF PREPARING THE SAME

Номер: US20130123538A1
Автор: Suzuki Yuji
Принадлежит: SUMITOMO BAKELITE CO., LTD.

According to the present invention, a liquid phenol resin that has excellent characteristics of a phenol resin, such as thermal resistance and hardenability, and can produce a molded product having excellent flexibility, and a method of preparing the resin are provided. 1. A liquid phenol resin obtained by reacting (A) oils and (B) phenols with (C) a secondary and/or a tertiary alkylamine compound.2. The liquid phenol resin according to claim 1 , wherein the (A) oils include at least one or more kinds selected from the group consisting of cashew oil claim 1 , linseed oil claim 1 , tung oil claim 1 , castor oil claim 1 , and tall oil.3. The liquid phenol resin according to claim 1 , wherein a nitrogen content based on the whole liquid phenol resin is 3% by weight to 30% by weight.4. The liquid phenol resin according to claims 1 , wherein a weight ratio between the (A) oils and the (B) phenols is (A):(B)=10:90 to 90:10.5. The liquid phenol resin according to claim 1 , wherein the (C) secondary and/or tertiary alkylamine compound includes hexamethylenetetramine.6. The liquid phenol resin according to claim 1 , which is obtained by reacting the (A) oils and the (B) phenols with the (C) secondary and/or a tertiary alkylamine compound claim 1 , in a molar ratio of (C)/{(A)+(B)}=0.13 to 0.35.7. The liquid phenol resin according to claim 1 , which is used for impregnation.8. A method of preparing a liquid phenol resin which is the liquid phenol resin according to claim 1 , comprising reacting (A) oils and (B) phenols with (C) a secondary and/or a tertiary alkylamine compound without performing a step of dehydration. The present invention relates to a liquid phenol resin and a method of preparing the same.Priority is claimed on Japanese Patent Application No. 2010-167934, filed Jul. 27, 2010, the content of which is incorporated herein by reference.A phenol resin as a thermosetting resin is widely used mainly as a binder for binding materials that become a substrate of a ...

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16-05-2013 дата публикации

METHOD FOR PRODUCING 2,5-DIAMINOTOLUENE

Номер: US20130123540A1
Автор: Aeby Johann, Goettel Otto
Принадлежит: ALFA PARF GROUP S.P.A.

The invention relates to a method for producing 2,5-diaminotoluene by catalytic hydrogenation in an aprotic-non-polar solvent or in a mixture made of two or more aprotic-nonpolar solvents with hydrogen in the presence of a catalyst or a mixture of two or more catalysts. The invention further relates to crystalline 2,5-diaminotoluene having characteristic crystal modification. As compared to conventional forms of administration common in industry, this is characterised in that it is largely insensitive to air oxidation. 1. A method for producing 2 ,5-diaminotoluene , comprising hydrogenating 2-methyl-4-nitroaniline in an aprotic nonpolar solvent or in a mixture made of two or more aprotic nonpolar solvents with hydrogen in the presence of a catalyst or a mixture made of two or more catalysts , thereby forming a solution containing 2 ,5-diaminotoluene and an aprotic nonpolar solvent or a mixture made of two or more aprotic nonpolar solvents.2. The method according to claim 1 , wherein the aprotic nonpolar solvent or the mixture made of two or more aprotic nonpolar solvents has a dielectric constant ∈in the range of 2.3 to 6.1.3. The method according to claim 1 , wherein the catalyst is a solid catalyst or the mixture made of two or more catalysts is a mixture containing at least one solid catalyst.4. The method according to claim 1 , wherein the catalyst is a palladium/activated carbon catalyst or the mixture made of two or more catalysts is a mixture containing at least one palladium/activated carbon catalyst.5. The method according to claim 1 , wherein the 2-methyl-4-nitroaniline is hydrogenated in a temperature range of 0° C. to 150° C.6. The method according to claim 1 , wherein the 2-methyl-4-nitroaniline is hydrogenated at a hydrogen overpressure in the range of 0 to 5 MPa.7. The method according to claim 1 , wherein at least one of the following steps is carried out after the hydrogenation:separating the catalyst or the mixture made of two or more catalysts ...

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16-05-2013 дата публикации

METHOD OF PREPARING 3,3,5,5-TETRAMETHYLCYCLOHEXANONE

Номер: US20130123541A1
Принадлежит: Merz Pharma GmbH & Co. KGaA

Method of preparing 3,3,5,5-tetramethylcyclohexanone comprising step (i): (i) converting isophorone to 3,3,5,5-tetramethylcyclohexanone in the presence of methylmagnesium chloride. The thus prepared 3,3,5,5-tetramethylcyclohexanone may be employed in a method of preparing 1-amino-1,3,3,5,5-pentamethylcyclohexane (Neramexane) or a pharmaceutically acceptable salt thereof. 116.-. (canceled)17. A method of preparing 3 ,3 ,5 ,5-tetramethylcyclohexanone comprising step (i):(i) converting isophorone to 3,3,5,5-tetramethylcyclohexanone in the presence of methylmagnesium chloride.18. The method according to claim 17 , wherein step (i) is performed in the presence of a copper compound.19. The method according to claim 18 , wherein the copper compound is a copper(I) halide.20. The method according to claim 19 , wherein the copper(I) halide is copper(I) iodide.21. The method according to claim 17 , wherein step (i) performed in the presence of a lithium compound.22. The method according to claim 21 , wherein the lithium compound is a lithium halide claim 21 ,23. The method according to claim 22 , wherein the lithium halide is lithium chloride.24. The method according to claim 22 , wherein the molar ratio of copper(I) halide to lithium halide is in the range of from 1:1.5 to 1:2.5.25. The method according to claim 17 , wherein step (i) is performed in a solvent comprising an ether.26. The method according to claim 25 , wherein the ether is tetrahydrofuran.27. The method according to claim 17 , wherein in step (i) isophorone is converted to 3 claim 17 ,3 claim 17 ,5 claim 17 ,5-tetramethylcyclohexanone in the presence of methylmagnesium chloride claim 17 , copper(I) iodide and lithium chloride in tetrahydrofuran.28. The method according to claim 27 , wherein a solution comprising methylmagnesium chloride in tetrahydrofuran is added to a solution comprising isophorone claim 27 , copper(I) iodide and lithium chloride.29. A method of preparing 1-amino-1 claim 27 ,3 claim 27 ,3 ...

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23-05-2013 дата публикации

METHOD FOR PRODUCING 2-CYANOACETIC ACID ANHYDRIDE AND FURTHER REACTION PRODUCTS THEREOF

Номер: US20130131370A1
Автор: Hynes Stephan
Принадлежит: Loctite (R&D) Limited Ltd.

The present invention relates to a process for producing 2-cyanoacetic acid anhydride, comprising the steps of a) preparing a reaction mixture, containing as reactants 2-cyanoacetic acid, and at least one Ccarboxylic acid anhydride in at least one organic solvent, wherein the molar ratio of 2-cyanoacetic acid to Ccarboxylic acid anhydride in said reaction mixture is greater than 1.5:1, and b) subjecting the reaction mixture to a temperature of 0° C. to 100° C. to form 2-cyanoacetic acid anhydride. The present invention also relates to process for producing 2-cyanoacetic acid esters, 2-cyanoacetic acid amides and/or 2-cyanoacetic acid thioesters from 2-cyanoacetic acid anhydride. 1. A process for producing 2-cyanoacetic acid anhydride , comprising the steps of:{'sub': 4-20', '4-20, 'a) preparing a reaction mixture, containing as reactants 2-cyanoacetic acid, and at least one Ccarboxylic acid anhydride in at least one organic solvent, wherein the molar ratio of 2-cyanoacetic acid to Ccarboxylic acid anhydride in said reaction mixture is greater than 1.5:1; and'}b) subjecting the reaction mixture to a temperature of 0° C. to 100° C. to form 2-cyanoacetic acid anhydride.2. The process of claim 1 , wherein the molar ratio of 2-cyanoacetic acid to Ccarboxylic acid anhydride in said reaction mixture is from 2:1 to 3:1.3. The process of claim 1 , wherein the Ccarboxylic acid anhydride is a symmetrical Ccarboxylic acid anhydride.6. The process according to claim 1 , wherein the Ccarboxylic acid anhydride is trifluoroacetic acid anhydride.7. The process according to claim 1 , wherein the temperature in step b) is from 10° C. to 40° C.8. The process of claim 1 , comprising the additional step c) of concentrating 2-cyanoacetic acid anhydride by removing at least a part of the organic solvent.9. A process for producing 2-cyanoacetic acid esters claim 1 , 2-cyanoacetic acid amides and/or 2-cyanoacetic acid thioesters claim 1 , comprising the steps of:{'claim-ref': {'@idref': 'CLM ...

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23-05-2013 дата публикации

METHOD FOR PRODUCING ISOCYANATES IN THE GAS PHASE

Номер: US20130131377A1
Принадлежит: Bayer Intellectual Property GmbH

The invention relates to a process for the preparation of isocyanates by reaction of the corresponding amines with phosgene in the gas phase, wherein a diluent containing between 90.0000% by weight and 99.9999% by weight of substances which are inert in the phosgenation process and between 0.0001% by weight and 10.0000% by weight of oxygen is present during the conversion of the amine into the gas phase and the molar ratio of amine to oxygen (O) is ≧1,000:1. 17.-. (canceled)8. Process for the preparation of isocyanates by reaction of the corresponding amines with phosgene in the gas phase , wherein(i) the amine is converted into the gas phase in a vaporization space in the presence of from >0.10% by weight to 25% by weight of a diluent, based on the total weight of diluent and amine;(ii) the gaseous stream obtained from (i) containing amine and diluent is reacted with a gaseous phosgene stream in a reaction space to give the corresponding isocyanate; the diluent employed in step (i) contains between 90.0000% by weight and 99.9999% by weight of substances which are inert in the phosgenation process and between 0.0001% by weight and 10.0000% by weight of oxygen, in each case based on the weight of the diluent, and', {'sub': '2', 'the molar ratio of amine to oxygen (O) in step (i) in the vaporization space is ≧1,000:1.'}], 'characterized in that'}9. Process according to claim 8 , in which in step (i) the amine is converted into the gas phase in the presence of >0.10% by weight to 10% by weight of a diluent which contains between 99.0000% by weight and 99.9950% by weight of substances which are inert in the phosgenation process and between 0.0050% by weight and 1.0000% by weight of oxygen claim 8 , in each case based on the weight of the diluent claim 8 , and wherein the molar ratio of amine to oxygen in the vaporization space is in the range between 1.000:1 and 1 claim 8 ,000 claim 8 ,000:1.10. Process according to claim 8 , in which in step (i) the amine is converted ...

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23-05-2013 дата публикации

Process for Preparing Ethylamines and Monoisopropylamine (MIPA)

Номер: US20130131385A1
Принадлежит: BASF SE

A process for preparing ethylamines and monoisopropylamine (MIPA), in which bioethanol is reacted with ammonia in the presence of hydrogen and of a heterogeneous catalyst to give ethylamines, said bioethanol having a content of sulfur and/or sulfur compounds of ≧0.1 ppm by weight (calculated S), and then isopropanol is reacted with ammonia in the presence of the same catalyst and in the presence of hydrogen to give MIPA. 124.-. (canceled)25. A process for preparing ethylamines and monoisopropylamine (MIPA) , which comprises reacting bioethanol with ammonia in the presence of hydrogen and of a heterogeneous catalyst to give ethylamines , said bioethanol having a content of sulfur and/or sulfur compounds of ≧0.1 ppm by weight (calculated S) , and then reacting isopropanol with ammonia in the presence of the same catalyst and in the presence of hydrogen to give MIPA.26. The process according to claim 25 , wherein the sulfur content of the catalyst at the end of the period over which the reaction of bioethanol with ammonia is performed is <700 ppm by weight.27. The process according to claim 25 , wherein the reactions are performed in the presence of a heterogeneous copper and/or nickel and/or cobalt catalyst.28. The process according to claim 25 , wherein the reactions are performed in the presence of a heterogeneous catalyst having a nickel content of more than 90% by weight claim 25 , based on any and all metals of group VIII of the Periodic Table present.29. The process according to claim 25 , wherein the reactions are performed in the presence of a heterogeneous catalyst having a cobalt content of more than 90% by weight claim 25 , based on any and all metals of group VIII of the Periodic Table present.30. The process according to claim 25 , wherein the reactions are performed in the presence of a heterogeneous copper and nickel catalyst.31. The process according to claim 25 , wherein the reactions are performed in the presence of a heterogeneous copper and nickel ...

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23-05-2013 дата публикации

BRANCHED SECONDARY ALCOHOL ALKOXYLATE SURFACTANTS FOR TEXTILE PROCESSING

Номер: US20130131386A1
Принадлежит: Dow Global Technologies LLC

Provided is a composition that is useful for textile processing, including for softening and providing smoothness to textiles The composition comprises an alkoxylate of the formula (I): wherein AO, EO, m, n, R. Rand Rare as defined below, and a polysiloxane oil 2. A composition according to wherein the polydispersity index of the alkoxylate is 1.15 or less.32. A composition according to any one of - wherein the composition comprises no more than 2 percent by weight of residual alcohol.43. A composition according to any one of - wherein AO is propyleneoxy or butyleneoxy.54. A composition according to any one of - wherein the group formed by R claims 1 , R claims 1 , Rand the carbon to which they are attached contains 9 to 12 carbon atoms.76. A composition according to any one of - wherein the polysiloxane oil is aminofunctionalized silicone oil claims 1 , amidofunctional silicone claims 1 , dimethylsilicone oil claims 1 , or hydroxyfunctional silicone.87. A composition according to any one of - where the composition is in the form of a concentrate.97. A composition according to any one of - where the composition further comprises water and is the form of an emulsion.10. A composition according to comprising 5 to 100 parts by weight of the alkoxylate and 20 to 2000 parts by weight of water claim 9 , based on 100 parts by weight of the polysiloxane oil.1110. A method for treating and processing textile materials which comprises contacting the textile materials with a composition according to any one of -.12. A textile treated by the method of . The invention relates to new branched secondary alcohol alkoxylates, to compositions thereof, and to their use in textile processing.Polysiloxanes are used in the textile processing industry as finishing agents for improving various properties of the textile, such as smoothness and softness. Typically, the polysiloxanes are employed in the form of oil-in-water emulsions, prepared by emulsification of a polysiloxane using a ...

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30-05-2013 дата публикации

PROCESS FOR PREPARING ISOCYANATES BY PHOSGENATION OF THE CORRESPONDING AMINES IN THE GAS PHASE

Номер: US20130137892A1
Принадлежит:

A process for preparing isocyanates by phosgenation of the corresponding amines in a fluidized-bed reactor (R), wherein a gas stream () comprising the phosgene is used as fluidizing gas and keeps an inert solid in suspension and a liquid stream () comprising the amine is fed into the fluidized bed, with the amine vaporizing partially or completely and reacting with the phosgene to give a reaction gas mixture which comprises the corresponding isocyanate and is taken off from the fluidized-bed reactor (R) is proposed. 1. A process for preparing isocyanates by phosgenation of the corresponding amines in a fluidized-bed reactor (R) , wherein{'b': '1', 'a gas stream () comprising the phosgene is used as fluidizing gas and keeps an inert solid in suspension and'}{'b': '2', 'a liquid stream () comprising the amine is fed into the fluidized bed,'}with the amine vaporizing partially or completely and reacting with the phosgene to give a reaction gas mixture which comprises the corresponding isocyanate and is taken off from the fluidized-bed reactor (R).2. The process according to claim 1 , wherein the fluidized-bed reactor (R) is a rotationally symmetrical apparatus having a vertical longitudinal axis.3. The process according to claim 2 , wherein the fluidized-bed reactor (R) is a predominantly cylindrical apparatus.41. The process according to any of to claim 2 , wherein the phosgene-comprising gas stream () comprising from 50 to 100% by weight of phosgene claim 2 , based on the total weight of the phosgene-comprising gas stream claim 2 , preferably from 75 to 100% by weight of phosgene claim 2 , based on the total weight of the phosgene-comprising gas stream claim 2 , more preferably from 90 to 99.9% by weight of phosgene claim 2 , based on the total weight of the phosgene-comprising gas stream claim 2 , is heated to a temperature which is at least 5° C. greater than the vaporization temperature of the amine under the operating conditions (pressure) in the fluidized-bed ...

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30-05-2013 дата публикации

Novel method of preparing secondary amine compound using microflow reactor

Номер: US20130137900A1

Disclosed is a novel method of preparing a secondary amine compound using a microflow reactor. According to the method, a primary amine compound and a halide compound are allowed to react with each other in the microflow reactor, such that the production of a tertiary amine compound or an ammonium salt is minimized, whereby the secondary amine compound is efficiently prepared.

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30-05-2013 дата публикации

SYNTHESIS OF POLYALKYLENEPOLYAMINES HAVING A LOW COLOR INDEX BY HOMOGENEOUSLY CATALYZED ALCOHOL AMINATION IN THE PRESENCE OF HYDROGEN

Номер: US20130137901A1
Принадлежит:

Process for the preparation of polyalkylenepolyamines by homogeneously catalyzed alcohol amination, in which aliphatic amino alcohols are reacted with one another or aliphatic diamines or polyamines are reacted with aliphatic diols or polyols with the elimination of water in the presence of a homogeneous catalyst and in the presence of hydrogen gas. Polyalkylenepolyamines obtainable by such processes and polyalkylenepolyamines comprising hydroxy groups, secondary amines or tertiary amines. Uses of such polyalkylenepolyamines as adhesion promoters for printing inks, adhesion promoters in composite films, cohesion promoters for adhesives, crosslinkers/curing agents for resins, primers for paints, wet-adhesion promoters for emulsion paints, complexing agents and flocculating agents, penetration assistants in wood preservation, corrosion inhibitors, immobilizing agents for proteins and enzymes. 1. A process for the preparation of polyalkylenepolyamines by homogeneously catalyzed alcohol amination , in which(i) aliphatic amino alcohols are reacted with one another or(ii) aliphatic diamines or polyamines are reacted with aliphatic diols or polyols with the elimination of water in the presence of a homogeneous catalyst and in the presence of hydrogen gas.2. The process according to claim 1 , wherein the reaction is carried out at a partial pressure of the hydrogen gas of from 0.1 to 25 MPa.3. The process according to or claim 1 , wherein the hydrogen gas engages chemically in the catalyzed alcohol amination claim 1 , thereby reducing the formation of coloring components.4. The process according to to claim 1 , wherein the catalyst is a transition metal complex catalyst.5. The process according to to claim 1 , wherein the catalyst comprises ruthenium or iridium.6. The process according to to claim 1 , wherein the catalyst comprises a nitrogen-heterocyclic carbene ligand.7. The process according to claim 6 , wherein the catalyst comprises a carbene ligand from the group ...

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06-06-2013 дата публикации

PROCESSES FOR PRODUCING DIAMINOBUTANE (DAB), SUCCINIC DINITRILE (SDN) AND SUCCINAMIDE (DAM)

Номер: US20130144028A1
Принадлежит:

Processes include providing a clarified diammonium succinate (DAS)- or monoammonium succinate (MAS)- containing fermentation broth; distilling the broth of an overhead that includes water and ammonia, and a liquid bottoms that includes SA, and at least about 20 wt % water; cooling the bottoms to a temperature sufficient to cause the bottoms to separate into a liquid portion in contact with a solid portion that is substantially pure SA; separating the solid portion from the liquid portion; and converting the solid portion to produce nitrogen containing compounds such as diamino butane (DAB), succinic dinitrile (SDN), succinic amino nitrile (SAN) or succinamide (DAM) and downstream products. 1. A process for making nitrogen containing compounds of SA comprising:(a) providing a clarified DAS-containing fermentation broth;(b) distilling the broth under super atmospheric pressure at a temperature of >100° C. to about 250° C. to form an overhead that comprises water and ammonia, and a liquid bottoms that comprises SA, and at least about 20 wt % water;(c) cooling and/or evaporating the bottoms to attain a temperature and composition sufficient to cause the bottoms to separate into a liquid portion and a solid portion that is substantially pure SA;(d) separating the solid portion from the liquid portion;(e) (1) contacting at least as part of the solid portion with hydrogen and an ammonia source in the presence of at least one hydrogenation catalyst to produce DAB, (2) dehydrating at least part of the solid portion to produce SDN or (3) dehydrating at least part of the solid portion to produce DAM; and(f) recovering the DAB, SDN or DAM.2. A process for making nitrogen containing compounds of SA comprising:(a) providing a clarified DAS-containing fermentation broth;(b) adding an ammonia separating and/or water azeotroping solvent to the broth;(c) distilling the broth at a temperature and pressure sufficient to form an overhead that comprises water and ammonia, and a liquid ...

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06-06-2013 дата публикации

PROCESS FOR THE PREPARATION OF ISOCYANATES

Номер: US20130144081A1
Принадлежит: Bayer Intellectual Property GmbH

The invention relates to a process for the preparation of isocyanates in a system network comprising an isocyanate production plant, a chlorine production plant and a phosgene production plant, in which carbon dioxide formed as a by-product is partially to completely condensed out with the gaseous chlorine formed in the chlorine production plant and enters into the phosgene preparation process and, after the preparation of phosgene, the predominant part of the carbon dioxide formed is thereby sluiced out of the system network in gaseous form. 1. A process for preparing an isocyanate comprising the steps of{'b': 1', '16', '1, '(i) reacting a stream E comprising a primary amine with a phosgene-comprising stream P to form a product stream P, which comprises said isocyanate, hydrogen chloride, unreacted phosgene, and carbon oxides;'}{'b': 1', '2', '3, '(ii) separating the product stream P into a liquid product stream P comprising said isocyanate and a gaseous product stream P comprising hydrogen chloride, unreacted phosgene, and carbon oxides;'}{'b': 3', '4', '5, '(iii) mixing the product stream P with a gaseous product stream P comprising oxygen to form a gaseous mixed stream P;'}{'b': 5', '6, '(iv) oxidizing the gaseous mixed stream P on a catalyst to form a gaseous product stream P comprising hydrogen chloride, carbon dioxide, excess oxygen, chlorine, and water;'}{'b': 6', '7', '8, '(v) partially to completely removing the hydrogen chloride and water from stream P as a stream P comprising hydrochloric acid to form a product stream P depleted in hydrogen chloride and water;'}{'b': 8', '9', '10', '8', '9, '(vi) separating the product stream P into a liquid chlorine-rich product stream P, which comprises chlorine, carbon dioxide, and oxygen, and a gaseous, low-chlorine product stream P, which comprises the residual amount of chlorine from P not contained in P, carbon dioxide, and oxygen;'}{'b': 10', '11', '12, '(vii) dividing the gaseous product stream P into a gaseous ...

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13-06-2013 дата публикации

SHREDDER WITH THICKNESS DETECTOR

Номер: US20130146693A1
Принадлежит: Fellowes, Inc.

A shredder is disclosed. The shredder includes a housing having a throat for receiving at least one article to be shredded, and a shredder mechanism received in the housing and including an electrically powered motor and cutter elements. The shredder mechanism enables the at least one article to be shredded to be fed into the cutter elements. The motor is operable to drive the cutter elements so that the cutter elements shred the articles fed therein. The shredder also includes a detector that is configured to detect a thickness of the at least one article being received by the throat, and a controller that is operable to perform a predetermined operation responsive to the detector detecting that the thickness of the at least one article is at least equal to a predetermined maximum thickness. 1a shredding mechanism with at least one blade capable of shredding paper;a delivery mechanism configured to deliver an agent to the at least one blade; anda reservoir in communication with the delivery mechanism, the delivery mechanism selectively drawing the agent from the reservoir for delivering the agent to the at least one blade of the shredding mechanism; anda mechanism that tracks the quantity of material passed through the shredder since the agent was last delivered to the shredding mechanism.. A paper shredder comprising: This application is a divisional of U.S. patent application Ser. No. 12/732,899, filed Mar. 26, 2010, which is a continuation of U.S. patent application Ser. No. 11/770,223, filed Jun. 28, 2007, now U.S. Pat. No. 7,712,689, which is a divisional application of U.S. patent application Ser. No. 11/444,491, filed Jun. 1, 2006, now U.S. Pat. No. 7,631,822, which is a continuation-in-part of U.S. patent application Ser. No. 11/177,480, filed Jul. 11, 2005, now U.S. Pat. No. 7,661,614, the entire contents of each of which are incorporated herein by reference with priority claimed. This application is also a divisional of U.S. patent application Ser. No. 12 ...

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13-06-2013 дата публикации

VERTICAL MILL

Номер: US20130146694A1
Принадлежит:

In a vertical mill, a pulverization table () is supported with a vertical rotation axis core in a housing () so as to be capable of being driven and rotated, and a pulverization roller () rotatable in conjunction with rotation of the pulverization table () is disposed above the pulverization table () so as to be opposed to the pulverization table (), and a cutter roller () rotatable in conjunction with rotation of the pulverization table () is disposed above the pulverization table () so as to be opposed to the pulverization table (). Accordingly, a solid matter such as biomass can be efficiently pulverized, thereby achieving improvement in pulverization efficiency. 1. A vertical mill , comprising:a pulverization table being supported with a vertical rotation axis core in a housing so as to be driven and rotated;a pulverization roller that is disposed above the pulverization table so as to be opposed to the pulverization table and is rotatable in conjunction with rotation of the pulverization table; anda cutter roller that is disposed above the pulverization table so as to be opposed to the pulverization table and is rotatable in conjunction with rotation of the pulverization table.2. The vertical mill according to claim 1 , whereina plurality of the pulverization rollers is disposed at regular intervals along a direction of rotation of the pulverization table, anda plurality of the cutter rollers is disposed so that each of the plurality of the cutter rollers is located next to each of the plurality of the pulverization rollers in the direction of rotation of the pulverization table.3. The vertical mill according to claim 1 , whereinthe housing includes a support shaft with a leading end part facing a rotation axis core of the pulverization table,the pulverization roller is rotatably supported at the support shaft, andthe cutter roller is rotatably supported at the support shaft.4. The vertical mill according to claim 3 , whereinthe pulverization roller is ...

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13-06-2013 дата публикации

SOLID DAPOXETINE

Номер: US20130150453A1
Принадлежит: SYMED LABS LIMITED

The present invention relates to solid racemic dapoxetine, solid dapoxetine S(+)enantiomer, processes for their preparation and their use in the pharmaceutically active compound dapoxetine acid addition salt, and pharmaceutical compositions thereof. 110-. (canceled)11. A solid racemic dapoxetine.12. A process for preparing solid racemic dapoxetine comprising:a) providing a solution of racemic dapoxetine in a hydrocarbon solvent n-hexane or cyclohexane or a mixture thereof; andb) evaporating the solvent(s), or by cooling the solution obtained in step (a) to below about 30° C. to obtain a solid; andc) recovering the solid obtained in step (b) by conventional methods to afford the desired racemic dapoxetine.13. The process of claim 12 , wherein the solution in step (a) is obtained by dissolving an oily residue or crude faun of racemic dapoxetine or racemic dapoxetine obtained from a reaction mixture of racemic dapoxetine or a salt thereof in a suitable organic solvent(s).14. The process of claim 12 , wherein the solution is obtained at a temperature range from about 30° C. to about the boiling point of the solvent (s) used.15. The process of claim 12 , wherein the solid is precipitated in step b) by evaporation of the solvents from the solution of step a) at elevated temperatures under reduced pressure or by cooling the solution from about −5° C. to about 30° C.16. The process of claim 12 , wherein recovery of solid racemic dapoxetine in step c) is by a conventional method.17. The process of claim 12 , wherein the solid racemic dapoxetine obtained is dried at a temperature range from about 25° C. to about 45° C. under reduced pressure.18. The process of claim 12 , wherein the solid racemic dapoxetine obtained is optionally recrystallized from a solvent or a mixture of solvents selected from the group consisting of esters claim 12 , alcohols claim 12 , or alcohols in combination with water in any proportion.19. A solid dapoxetine S(+) enantiomer.20. process for ...

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13-06-2013 дата публикации

Method for Producing Primary Aliphatic Amines from Aldehydes

Номер: US20130150624A1
Принадлежит: OXEA GMBH

A continuous process for producing primary aliphatic amines having 9 to 18 carbon atoms by reaction of corresponding aliphatic aldehydes with ammonia and hydrogen in the presence of a hydrogenation catalyst in the liquid phase, characterized in that the reaction is carried out solventlessly at a molar ratio of aliphatic aldehyde:ammonia of at least 1:30, at a temperature of 100 to 200° C. and at a pressure of 6 to 11 MPa. 1. Continuous process for producing primary aliphatic amines having 9 to 18 carbon atoms by reaction of corresponding aliphatic aldehydes with ammonia and hydrogen in the presence of a hydrogenation catalyst in the liquid phase , characterized in that the reaction is carried out solventlessly at a molar ratio of aliphatic aldehyde:ammonia of at least 1:30 , at a temperature of 100 to 200° C. and at a pressure of 6 to 11 MPa.2. Process according to claim 1 , characterized in that the molar ratio of aliphatic aldehyde:ammonia is at least 1:35.3. Process according to claim 1 , characterized in that the reaction is carried out at a temperature of 100 to 170° C.4. Process according to claim 3 , characterized in that the reaction is carried out at a temperature of 120 to 150° C.5. Process according to claim 1 , characterized in that the reaction is carried out at a pressure of 7 to 9 MPa.6. Process according to claim 1 , characterized in that the aliphatic aldehydes to be reacted contain 9 to 15 carbon atoms in the molecule.7. Process according to claim 1 , characterized in that the hydrogenation catalyst contains at least nickel claim 1 , cobalt claim 1 , platinum claim 1 , palladium claim 1 , iron claim 1 , rhodium or copper.8. Process according to claim 1 , characterized in that the hydrogenation catalyst contains a support material.9. Process according to claim 1 , characterized in that the hydrogenation catalyst contains oxides of calcium claim 1 , of barium claim 1 , of zinc claim 1 , of aluminium claim 1 , of zirconium claim 1 , of chromium claim ...

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20-06-2013 дата публикации

PROCESS FOR THE SYNTHESIS OF 1-AMINO-3-HALO-4,6-DINITROBENZENE

Номер: US20130158296A1
Принадлежит: E I DU PONT DE NEMOURS AND COMPANY

A process is provided for the preparation of 1-amino-3-halo-4,6-dinitrobenzene and related compounds by monoamination of dihalodinitrobenzenes by ammonia in the presence of solvent and water. Using glycol as a solvent for the dihalodinitrobenzene and feeding ammonia at a rate at which it is consumed allows for the synthesis of high purity product, such as 1-amino-3-chloro-4,6-dinitrobenzene, at high yields. 2. A process according to wherein each Z is Cl.3. A process according to wherein Z═Cl and R claim 2 , R claim 2 , R claim 2 , and Rare each H.4. A process according to wherein the solvent comprises an aliphatic dihydric alcohol.5. A process according to wherein the aliphatic dihydric alcohol is ethylene glycol.6. A process according to wherein the reaction mixture is prepared by contacting a suspension of a compound represented by Formula (III) in solvent and water with gaseous ammonia.7. A process according to wherein the reaction mixture is prepared by contacting a suspension of a compound represented by Formula (III) in solvent with an aqueous solution of ammonia.8. A process according to wherein the reaction mixture is prepared by contacting a compound represented by Formula (III) with a feed stream containing solvent claim 1 , water and NH.9. A process according to wherein the amount of water is between about 1 and about 5 times the amount of NH.10. A process according to wherein the compound represented by Formula (II) thereby produced is filtered and washed with solvent and then water.11. A process according to wherein the filtrate containing solvent is collected and distilled claim 10 , and the solvent is recovered and recycled to the reaction mixture.12. A process according to wherein the compound represented by Formula (II) thereby produced is slurried with water as a suspension and transferred to another reactor for further processing. This application claims priority under 35 U.S.C. §119(e) from, and claims the benefit of, U.S. Provisional Application ...

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27-06-2013 дата публикации

PROCESS FOR THE DIRECT AMINATION OF SECONDARY ALCOHOLS WITH AMMONIA TO GIVE PRIMARY AMINES

Номер: US20130165672A1
Принадлежит: EVONIK DEGUSSA GmbH

The invention relates to a process for preparing primary amines which comprises the process steps 1. A process for preparing a primary amine , the process comprising:i) providing a solution of a secondary alcohol in a fluid, nongaseous phase, free ammonia, at least one ammonia-releasing compound, or both,', 'and a homogeneous catalyst, and, 'ii) contacting the solution with'} 'wherein:', 'iii) optionally isolating the primary amine obtained in said contacting ii),'}a) a volume ratio of a liquid phase to a gas phase in said contacting ii) is greater than or equal to 0.25, orb) a molar ratio of the ammonia to hydroxyl groups in the secondary alcohol is at least 5:1, orboth a) and b).2. The process according to claim 1 , wherein the homogeneous catalyst isan alkali metal alkoxide, an aluminium alkoxide, a lanthanide alkoxide, an inorganic compound of noble metals,a monometallic or multimetallic, mononuclear or multinuclear coordination compound of at least one noble metal selected from the group consisting of ruthenium, iridium, rhodium, osmium, palladium, platinum and iron,or any mixture thereof.3. The process according to claim 1 ,whereinthe secondary alcohol comprises at least two secondary hydroxy groups.4. The process according to claim 1 ,whereinthe secondary alcohol comprises a cyclic or polycyclic carbon skeleton.5. The process according to claim 1 ,whereinthe secondary alcohol is selected from the group consisting of:2-dodecanol, cyclododecanol, 4-phenyl-2-butanol, isosorbide, isomannide, isoidite, polypropylene glycol, mannitol, sorbitol, galactitol and an alkyl glycoside.6. The process according to claim 1 ,whereinthe secondary alcohol is selected from the group consisting of an alpha-hydroxycarboxylic acid and an OH-modified, natural fatty acid.7. The process according to claim 1 ,wherein a liquid or supercritical ammonia, a solution of ammonium salts in a solvent, or both is used in said contacting ii).8. The process according to claim 1 ,whereinsaid ...

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27-06-2013 дата публикации

NOVEL PROCESSES FOR THE PREPARATION OF PHENYLCYCLOPROPYLAMINE DERIVATIVES AND USE THEREOF FOR PREPARING TICAGRELOR

Номер: US20130165696A1
Принадлежит: ACTAVIS GROUP PTC EHF

Provided herein are novel processes for the preparation of phenylcyclopropylamine derivatives, which are useful intermediates in the preparation of triazolo[4,5-d]pyrimidine compounds. Provided particularly herein are novel, commercially viable and industrially advantageous processes for the preparation of a substantially pure ticagrelor intermediate, trans-(1R,2S)-2-(3,4-difluorophenyl)-cyclopropylamine. Provided further herein are novel acid addition salts of trans-(1R,2S)-2-(3,4-difluorophenyl)-cyclopropylamine, and process for their preparation. The intermediate and its acid addition salts are useful for preparing ticagrelor, or a pharmaceutically acceptable salt thereof, in high yield and purity. 2. The process of claim 1 , wherein the halogen atom ‘X’ in the compound of formula VII is Cl or Br; and wherein the halogen atom in the compounds of formulae II claim 1 , III claim 1 , IV claim 1 , VI and VIII is F.3. The process of claim 1 , wherein the halogen atom ‘X’ in the compound of formula VII is Br; and wherein the R claim 1 , Rand Rin the compounds of formulae II claim 1 , III claim 1 , IV claim 1 , VI and VIII are H claim 1 , and wherein the Rand Rare F.4. The process of claim 1 , wherein the first solvent used in step-(a) is selected from the group consisting of an ester claim 1 , a nitrile claim 1 , a hydrocarbon claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , a polar aprotic solvent claim 1 , and mixtures thereof; wherein the second solvent used in step-(b) is selected from the group consisting of a ketone claim 1 , an ester claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , and mixtures thereof; wherein the third solvent used in step-(c) is selected from the group consisting of water claim 1 , an alcohol claim 1 , a ketone claim 1 , a cyclic ether claim 1 , an aliphatic ether claim 1 , a hydrocarbon claim 1 , a chlorinated hydrocarbon claim 1 , a nitrile claim 1 , ...

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04-07-2013 дата публикации

Alpha-cyanoacrylate ester synthesis

Номер: US20130171092A1
Автор: Stephen Hynes
Принадлежит: Henkel Ireland Ltd, Monheim

The high temperatures required for cracking the cyanoacrylate oligomers, produced by the Knovenagel condensation of formaldehyde and a cyanoacetate, limit the synthetic diversity and the number of different side chains that can be incorporated into a cyanoacrylate prepared using this method. Accordingly, the diversity of cyanoacrylate monomers prepared industrially is quite limited. Disclosed herein is a method for the preparation of alpha-Cyanoacrylate ester monomers from a variety of phosphonium and ammonium alpha-cyanoacrylate salts. The phosphonium and ammonium alpha-cyanoacrylate salts are of the general formula:

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04-07-2013 дата публикации

PROCESSES FOR PRODUCING DIAMINOBUTANE (DAB), SUCCINIC DINITRILE (SDN) AND SUCCINAMIDE (DAM)

Номер: US20130172519A1
Принадлежит: BIOAMBER S.A.S.

Processes that make nitrogen-containing compounds include converting succinic acid (SA) or monoammonium succinate (MAS) derived from a diammonium succinate (DAS)- or MAS-containing fermentation broth to produce such compounds including diaminobutane (DAB), succinic dinitrile (SDN), succinic amino nitrile (SAN), succinamide (DAM), and related polymers. 1. A process for making nitrogen containing compounds , comprising:(a) providing a clarified DAS-containing fermentation broth;(b) distilling the broth to form an overhead that comprises water and ammonia, and a liquid bottoms that comprises MAS, at least some DAS, and at least about 20 wt % water;(c) cooling and/or evaporating the bottoms, and optionally adding an antisolvent to the bottoms, to attain a temperature and composition sufficient to cause the bottoms to separate into a DAS-containing liquid portion and a MAS-containing solid portion that is substantially free of DAS;(d) separating at least part of the solid portion from the liquid portion; (2) dehydrating at least a part of the solid portion to produce SDN; or', '(3) dehydrating at least a part of the solid portion to produce DAM; and, '(e) (1) contacting the solid portion with hydrogen and optionally an ammonia source in the presence of at least one hydrogenation catalyst to produce DAB; or'}(f) recovering the DAB, SDN or DAM.2. A process for making nitrogen containing compounds , comprising:(a) providing a clarified DAS-containing fermentation broth;(b) distilling the broth to form a first overhead that includes water and ammonia, and a first liquid bottoms that includes MAS, at least some DAS, and at least about 20 wt % water;(c) cooling and/or evaporating the bottoms, and optionally adding an antisolvent to the bottoms, to attain a temperature and composition sufficient to cause the bottoms to separate into a DAS-containing liquid portion and a MAS-containing solid portion that is substantially free of DAS;(d) separating the solid portion from the ...

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04-07-2013 дата публикации

INTEGRATED PROCESSES FOR THE PREPARATION OF POLYBENZIMIDAZOLE PRECURSORS

Номер: US20130172621A1
Принадлежит: E.I.DU PONT DE NEMOURS AND COMPANY

An integrated process is provided for efficiently preparing 2,4,5-triaminophenol, starting with nitration of 2,6-dihalobenzene; high purity salts thereof; and complexes of 2,4,5-triaminophenol aromatic diacids, which are precursors for making polybenzimidazole polymer for high performance fibers. The process design eliminates several costly intermediate drying and recrystallization steps. The handling of solid materials with possible skin sensitizing properties and toxicity is avoided, thereby eliminating human and environmental exposure. 2. The process of further comprising slurrying or dissolving the 2 claim 1 ,4 claim 1 ,5-triaminophenol product in water; adding an acid to the slurry to form and precipitate 2 claim 1 ,4 claim 1 ,5-triaminophenol salt; and cooling claim 1 , filtering claim 1 , and washing the precipitated 2 claim 1 ,4 claim 1 ,5-triaminophenol salt.3. The process of wherein the acid in step (j) is selected from the group consisting of HCl claim 1 , acetic acid claim 1 , HSO claim 1 , and HPO.4. The process of wherein Z═Cl and the acid in step (j) is HCl.5. The process of wherein the solvent used in step (e) is distilled and recycled.6. The process of wherein the spent hydrogenation catalyst of step (k) is recovered and recycled.7. The process of wherein the acid added to the slurry to form and precipitate 2 claim 2 ,4 claim 2 ,5-triaminophenol salt is selected from the group consisting of HCl claim 2 , acetic acid claim 2 , HSO claim 2 , and HPO.8. The process of wherein the precipitated salt is washed with water and methanol claim 2 , and the methanol is recycled.9. The process of further comprising drying the 2 claim 2 ,4 claim 2 ,5-triaminophenol salt.10. The process of further comprising adding a reducing agent to at least one aqueous suspension or aqueous solution containing 2 claim 1 ,4 claim 1 ,5-triaminophenol or 2 claim 1 ,4 claim 1 ,5-triaminophenol salt.11. The process of claim 10 , wherein the reducing agent is tin powder.12. The ...

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04-07-2013 дата публикации

PROCESS FOR MAKING TERTIARY AMINOALCOHOL COMPOUNDS

Номер: US20130172622A1
Принадлежит: ANGUS Chemical Company

Provided is a process for making a tertiary aminoalcohol compound. The process comprises using an excess amount of a carbonyl compound in a condensation step between the carbonyl compound and a nitroalkane, and conducting a hydrogenation/alkylation step to produce the tertiary aminoalcohol. The process uses fewer steps than conventional processes. 2. The process of wherein the intermediate product mixture of step (a) comprises at least two moles of free carbonyl compound of formula III per mole of nitroalcohol compound of formula II.3. The process of wherein additional carbonyl compound of formula III is added following step (b).4. The process of wherein Rand Rare each independently C-Calkyl.5. The process of wherein Rand Rare each —C(OH)RR.6. The process of wherein Ris —C(OH)RRand Ris C-Calkyl.7. The process of wherein Rand Rtogether with the carbon to which they are attached form C-Ccycloalkyl.8. The process of wherein Rand Rare H.9. The process of wherein following step (b) claim 1 , the concentration of the tertiary aminoalcohol compound of formula I in the intermediate product mixture is at least 0.5 percent by weight.10. The process of wherein the compound of formula I is 2-(dimethylamino)-2-methyl-1-propanol claim 1 , N claim 1 ,N-dimethyltris(hydroxymethyl)aminomethane claim 1 , 2-(dimethylamino)-2-ethylpropane-1 claim 1 ,3-diol claim 1 , 2-(dimethylamino)-2-methylpropane-1 claim 1 ,3-diol or 1-(dimethylamino)cyclohexylmethanol. The invention relates to an improved process for making tertiary aminoalcohol compounds.Tertiary aminoalcohol compounds play an important role in a variety of commercial and consumer products. For instance, they may be used as neutralizers in paints and coatings, in process water applications, and personal care and cosmetics formulations, as emulsifying agents, as corrosion inhibitors, e.g., in metalworking fluids, as resin solubilizers, foam catalysts, finish stabilizers, and/or as raw materials for chemical synthesis of other ...

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11-07-2013 дата публикации

MONOCATIONIC POLYHYDROXYL COMPOUNDS

Номер: US20130178542A1
Принадлежит: Dow Global Technologies LLC

Described are novel monocationic polyhydroxyl compounds and their uses in personal care compositions. 2. The compound of claim 1 , wherein Rand Rare each H.3. The compound of claim 1 , wherein Rand Rare each H.4. The compound of claim 1 , wherein Rand Rare each —CH.5. The compound of claim 1 , wherein Rand Rare each —CHCH(OH)CHOH.6. The compound of claim 1 , wherein Rand Rare each —CHCHOH.7. The compound of claim 1 , wherein Ris —(CH)CHand Ris —CHCHOH.8. The compound of claim 1 , wherein Ris —CHOH.9. The compound of claim 1 , wherein Ris —CHCH.10. The compound of claim 1 , wherein Rand Rcooperate to form a cyclohexyl group.12. A method for providing humectancy in a personal care composition claim 1 , comprising including the compound of into the personal care composition.13. A hair care composition containing the compound of .14. A skin care composition containing the compound of . The present invention relates to novel monocationic polyhydroxyl compounds and their uses in personal care compositions.Polyhydroxyl compounds, or polyols, have a number of uses, from raw materials used in the manufacture of urethane foams to humectants for personal care products like shaving foams, lotions, and shampoos.Quaternary ammonium compounds are also useful in a number of applications, such as for disinfectants, surfactants, fabric softeners, and conditioners in shampoos.Despite the number of available conventional compounds, there is a strong need for novel compounds with properties to differentiate performance or offer synergistic effects in areas of interest, particularly in personal care compositions.In one embodiment, the present invention provides compounds, including salts, of the Formula (I):wherein:The term “optionally substituted” as used herein means that the groups in question are either unsubstituted or substituted with one or more groups, radicals or moieties, selected from halogen, hydroxy, amino or carboxy. When the groups in question are substituted with more ...

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11-07-2013 дата публикации

High-speed mixing reactor and application thereof

Номер: US20130178596A1
Принадлежит: Yantai Wanhua Polyurethanes Co Ltd

Disclosed is a rapid mixing reactor, comprising a first feed-in passage housing, a reactor housing, a second feed-in passage, a hollow blade-wheel feed distributor, a rotation shaft, and a first feed distributor, wherein the first feed-in passage housing and the reactor housing are constructed coaxially and communicated with each other; the second feed-in passage, the hollow blade-wheel feed distributor and the rotation shaft each are fixed in connection with each other in the sequence along the central axis of the reactor; the hollow blade-wheel feed distributor is located within the reactor housing and rotates axially under the driving force of the rotation shaft; the second feed-in passage is connected with the hollow blade-wheel feed distributor; the first feed-in passage housing is set up with at least one first feed-in inlet therein; the reactor housing is set up with at least one reaction liquid outlet at its distal end; and the first feed distributor and the hollow blade-wheel feed distributor are provided with first feed-in jetting hole(s) and second feed-in jetting hole(s), respectively. The reactor is capable of effecting instantaneously rapid mixing of two streams of fluid under a massive capacity, and improving the yield and quality of the target product.

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11-07-2013 дата публикации

PROCESS FOR CINACALCET HYDROCHLORIDE

Номер: US20130178654A1
Принадлежит: HETERO RESEARCH FOUNDATION

3-[3-(Trifluoromethyl)phenyl]propionaldehyde is a key intermediate for the preparation of cinacalcet hydrochloride. The present invention provides a novel process for the preparation of 3-[3-(trifluoromethyl)phenyl]propionaldehyde. The present invention also provides an improved process for preparation of cinacalcet hydrochloride in high yields. The present invention further provides a process for purification of cinacalcet hydrochloride. 2. The process according to claim 1 , wherein the R′ is methyl or ethyl.3. (canceled)4. The process according to claim 1 , wherein the solvent used in the process is selected from the group consisting of cyclohexane claim 1 , cyclohexene claim 1 , cycloheptane claim 1 , cyclopentane claim 1 , n-hexane claim 1 , n-heptane claim 1 , benzene claim 1 , toluene claim 1 , xylene claim 1 , dichloromethane claim 1 , chloromethane claim 1 , dichloroethane claim 1 , chloroform claim 1 , carbon tetrachloride claim 1 , chlorobenzene claim 1 , tetrahydrofuran claim 1 , diisopropyl ether claim 1 , tertrahydropyran claim 1 , 1 claim 1 ,4-dioxane claim 1 , methyl tert-butyl ether claim 1 , ethyl tert-butyl ether claim 1 , diethyl ether claim 1 , di-tert-butyl ether claim 1 , diglyme claim 1 , dimethoxyethane claim 1 , dimethoxymethane methoxyethane claim 1 , and mixtures thereof.5. The process according to claim 4 , wherein the solvent is selected from the group consisting of n-hexane claim 4 , cyclohexane claim 4 , toluene claim 4 , dichloromethane claim 4 , diisopropyl ether claim 4 , and tetrahydrofuran claim 4 , and mixtures thereof.6. The process according to claim 5 , wherein the the solvent is selected from the group consisting of n-hexane claim 5 , toluene claim 5 , dichloromethane claim 5 , tetrahydrofuran claim 5 , and mixtures thereof.7. The process according to claim 1 , wherein the reaction mass is maintained in the process below −50° C.8. The process according to claim 7 , wherein the reaction mass is maintained at about −70 to −85° ...

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11-07-2013 дата публикации

METHOD FOR SYNTHESIZING 3,5-DICHLOROANISOLE FROM 1,3,5-TRICHLOROBENZENE

Номер: US20130178655A1

The invention relates to a method for synthesizing 3,5-dichloroanisole from 1,3,5-trichlorobenzene, which comprises: 1. A method for synthesizing 3 ,5-dichloro-anisole from 1 ,3 ,5-trichlorobenzene , which comprises:a) reacting 1,3,5-trichloro-benzene and with a methanolate of an alkaline or alkaline-earth metal in a first solvent selected from the group consisting of dimethylsulfoxide, 1,1,3,3-tetramethylurea and mixtures thereof;b) precipitating the product resulting from step a) in a second solvent which is not included among the substances considered to be carcinogenic, mutagenic and/or toxic for reproduction by Regulation (EC) n° 1272/2008 of the European Parliament and of the Council of 16 Dec. 2008; thenc) recovering the precipitate thus-obtained in b).2. The method according to claim 1 , wherein the first solvent is dimethylsulfoxide.3. The method according to claim 1 , wherein the methanolate is selected from the group consisting of the methanolates of sodium claim 1 , potassium claim 1 , lithium claim 1 , magnesium claim 1 , calcium and barium.4. The method according to claim 3 , wherein the methanolate is sodium methanolate.5. The method according to claim 1 , wherein the methanolate is used to the proportion of 1 to 3 molar equivalents relative to the 1 claim 1 ,3 claim 1 ,5-trichlorobenzene.6. The method according to claim 1 , wherein a) is conducted at a temperature of 40 to 120° C.7. The method according to claim 1 , wherein a) is conducted for a time ranging from 15 minutes to 24 hours.8. The method according to claim 1 , wherein the second solvent is water.9. The method according to claim 1 , which additionally further comprises the washing of the precipitate recovered at c) with a third solvent which is not included among the substances considered to be carcinogenic claim 1 , mutagenic and/or toxic for reproduction by Regulation (EC) n° 1272/2008 of the European Parliament and of the Council of 16 Dec. 2008.10. The method according to claim 9 , ...

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11-07-2013 дата публикации

PROCESS FOR PREPARING SECONDARY AMINES IN THE LIQUID PHASE

Номер: US20130178656A1
Принадлежит:

The present application relates to a process for preparing secondary amines by aminating excess primary or secondary alcohols with primary amines in the liquid phase in the presence of copper-comprising catalysts. 2. The process according to claim 1 , excluding secondary amines of the formula I which are prepared from 1-dodecanol as the compound of the formula II with monomethylamine as the compound of the formula III.3. The process according to either of and claim 1 , wherein R claim 1 , Rand Rare each selected from the group of linear or branched aliphatic radicals having 1 to 4 carbon atoms.4. The process according to any of to claim 1 , wherein the catalyst precursor comprising copper oxides comprises 1 to 80% by weight of copper oxide.5. The process according to any of to claim 1 , wherein the catalyst support used comprises aluminum oxides claim 1 , silicon dioxide claim 1 , titanium dioxides claim 1 , zirconium dioxide claim 1 , lanthanum oxide claim 1 , molybdenum oxide claim 1 , tungsten oxide or mixtures of these oxides.6. The process according to any of to claim 1 , excluding hydrogenation catalysts which claim 1 , as well as copper claim 1 , also comprise tungsten and/or molybdenum as a metal and/or in the form of the oxides thereof.7. The process according to any of to claim 1 , wherein the catalyst support used is aluminum oxide and/or lanthanum oxide.8. The process according to to claim 1 , wherein the molar ratio of alcohol II to primary amine III is 1.5 to 15:1.9. The process according to claim 1 , wherein the hydrogenation output after step (ii) is subjected to the following workup steps:(a) distillatively removing alcohol II, optionally amine of the formula III and a portion of the water from the hydrogenation output,(b) extracting the hydrogenation output which has been obtained from (a) and freed of alcohol II, optionally amine of the formula III and a portion of the water with an aqueous alkali metal and/or alkaline earth metal hydroxide ...

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18-07-2013 дата публикации

ANTI-MICROBIAL AND ANTI-STATIC SURFACE TREATMENT AGENT WITH QUATERNARY AMMONIUM SALT AS ACTIVE INGREDIENT AND METHOD FOR PREVENTING STATIC ELECTRICITY IN POLYMER FIBERS USING SAME

Номер: US20130183456A1
Автор: KIM Seong Cheol

Provided are an anti-static and anti-microbial surface treatment agent including a quaternary ammonium salt compound as an active ingredient and a method of preventing a polymer fiber from developing static electricity by using the surface treatment agent. The quaternary ammonium salt compound has excellent anti-static and anti-microbial effects for the prevention or improvement of static electricity in a polymer fiber. Accordingly, the quaternary ammonium salt compound is suitable for use as a fabric softener, or an anti-static agent, and also, provides anti-microbial effects to a polymer fiber. 2. A method of preventing static electricity in a polymer fiber claim 1 , comprising treating the polymer fiber with a surface treatment agent of .3. The method of claim 1 , wherein the method comprises: dipping the polymer fiber in a solvent; and treating the polymer fiber with the surface treatment agent of and a reaction catalyst.4. The method of claim 3 , wherein the reaction catalyst is treated at room temperature.5. The method of claim 3 , further comprising claim 3 , prior to the treating the polymer fiber with the surface treatment agent of claim 3 , forming a radical of the polymer fiber by using at least one treatment selected from (i) a treatment with a reaction catalyst claim 3 , (ii) irradiation of gamma ray claim 3 , (iii) irradiation of E-beam claim 3 , (iv) irradiation of ion-beam claim 3 , (v) irradiation of deep ultra violet (UV) light claim 3 , and (vi) a plasma treatment.6. The method of claim 5 , comprisingforming a radical of the polymer fiber by using at least one treatment selected from (i) a treatment with a reaction catalyst, (ii) irradiation of gamma ray, (iii) irradiation of E-beam, (iv) irradiation of ion-beam, (v) irradiation of deep ultra violet (UV) light, and (vi) a plasma treatment; and{'claim-ref': {'@idref': 'CLM-00001', 'claim 1'}, 'adding the surface treatment agent of to the radical of the polymer fiber to form a covalent bond with a ...

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18-07-2013 дата публикации

Method for Allylating and Vinylating Aryl, Heteroaryl, Alkyl, and Alkene Halogenides Using Transition Metal Catalysis

Номер: US20130184485A1
Принадлежит: Saltigo GmbH

What is described is a process for preparing organic compounds of the general formula (I) 2. The process as claimed in preceding claim 1 , characterized in that R is an optionally substituted alkenyl claim 1 , alkyl claim 1 , aryl or heteroaryl radical claim 1 , where the heteroaryl radical is a five- claim 1 , six- or seven-membered ring having one or more nitrogen claim 1 , oxygen and/or sulfur atoms in the ring claim 1 , where any further optionally substituted aromatic claim 1 , heteroaromatic and/or cycloaliphatic radicals may be fused onto a cyclic R radical and the R radical may optionally bear one or more substituents which may each independently be (C-C)-alkyl claim 1 , (C-C)-cycloalkyl claim 1 , (C-C)-alkenyl claim 1 , (C-C)-cycloalkenyl claim 1 , (C-C)-alkynyl claim 1 , (C-C)-aryl claim 1 , O—[(C-C)-alkyl] claim 1 , O—[(C-C)-aryl] claim 1 , O—Si[(C-C)-alkyl][(C-C)-aryl] claim 1 , OC(O)—[(C-C)-alkyl] claim 1 , OC(O)—[(C-C)-aryl] claim 1 , NH claim 1 , NH[(C-C)-alkyl] claim 1 , N[(C-C)-alkyl] claim 1 , NH[(C-C)-aryl] claim 1 , N[(C-C)-aryl] claim 1 , NHC(O)—[(C-C)-alkyl] claim 1 , N[(C-C)-alkyl]C(O)—[(C-C)-alkyl] claim 1 , NHC(O)—[(C-C)-aryl] claim 1 , N[(C-C)-alkyl]C(O)—[(C-C)-aryl] claim 1 , NO claim 1 , NO claim 1 , S—[(C-C)-aryl] claim 1 , S—[(C-C)-alkyl] claim 1 , fluorine claim 1 , chlorine claim 1 , bromine claim 1 , pentafluorosulfuranyl claim 1 , CF claim 1 , CN claim 1 , COOM claim 1 , COO—[(C-C)-alkyl] claim 1 , COO—[(C-C)-aryl] claim 1 , C(O)NH—[(C-C)-alkyl] claim 1 , C(O)NH—[(C-C)-aryl] claim 1 , C(O)N—[(C-C)-alkyl] claim 1 , C(O)N—[(C-C)-aryl] claim 1 , CHO claim 1 , SO—[(C-C)-alkyl] claim 1 , SO—[(C-C)-alkyl] claim 1 , SO—[(C-C)-aryl] claim 1 , OSO—[(C-C)-alkyl] claim 1 , OSO—[(C-C)-aryl] claim 1 , PO—[(C-C)-alkyl] claim 1 , PO—[(C-C)-aryl] claim 1 , SOM claim 1 , SO—[(C-C)-alkyl] claim 1 , SO—[(C-C)-aryl] or Si[(C-C)-alkyl][(C-C)-aryl] claim 1 , where M is an alkali metal or alkaline earth metal atom and n is a natural number in the range ...

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18-07-2013 дата публикации

PROCESS FOR PRODUCTION OF HEXAMETHYLENEDIAMINE FROM CARBOHYDRATE-CONTAINING MATERIALS AND INTERMEDIATES THEREFOR

Номер: US20130184495A1
Принадлежит: Rennovia, Inc.

Processes are disclosed for the conversion of a carbohydrate source to hexamethylenediamine (HMDA) and to intermediates useful for the production of hexamethylenediamine and other industrial chemicals. HMDA is produced by direct reduction of a furfural substrate to 1,6-hexanediol in the presence of hydrogen and a heterogeneous reduction catalyst comprising Pt or by indirect reduction of a furfural substrate to 1,6-hexanediol wherein 1,2,6-hexanetriol is produced by reduction of the furfural substrate in the presence of hydrogen and a catalyst comprising Pt and 1,2,6-hexanediol is then converted by hydrogenation in the presence of a catalyst comprising Pt to 1,6 hexanediol, each process then proceeding to the production of HMDA by known routes, such as amination of the 1,6 hexanediol. Catalysts useful for the direct and indirect production of 1,6-hexanediol are also disclosed. 1. A process for preparing hexamethylenediamine from a carbohydrate source , the process comprising: converting a carbohydrate source to a furfural substrate; reacting at least a portion of the furfural substrate with hydrogen in the presence of a heterogeneous reduction catalyst to produce 1 ,6-hexanediol; and , converting at least a portion of the 1 ,6-hexanediol to hexamethylenediamine.2. The process of claim 1 , wherein the heterogeneous reduction catalyst comprises Pt.3. The process of claim 2 , wherein the heterogeneous reduction catalyst further comprises a support selected from the group consisting of zirconias claim 2 , silicas claim 2 , and zeolites.4. The process of claim 2 , wherein the heterogeneous reduction catalyst further comprises at least one metal selected from the group consisting of Mo claim 2 , La claim 2 , Sm claim 2 , Y claim 2 , W claim 2 , and Re.5. The process of claim 1 , wherein the reaction of the furfural substrate with hydrogen is carried out at a temperature in the range of about 60° C. and about 200° C. and a pressure of hydrogen in the range of about 200 psig ...

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25-07-2013 дата публикации

NOVEL COMPOUND ACCELERATING SECRETION OF HUMAN-DERIVED ANTI-MICROBIAL PEPTIDE, METHOD FOR PREPARING SAME, AND COMPOSITION HAVING SAME AS ACTIVE INGREDIENT

Номер: US20130190397A1
Принадлежит: NEOPHARM CO., LTD.

Disclosed is a compound having an acceleration effect on the secretion of human β-defensin, LL-37, which is a human-derived anti-microbial peptide, a method for preparing same, and a composition for accelerating the secretion of anti-microbial peptide having same as an active ingredient, and the compound and the composition using same of the present invention enhance the anti-microbial effect and the immunity control effect that the anti-microbial peptide has in the body by accelerating the secretion of the anti-microbial peptide in the body. 18-. (canceled)10. The new compound of claim 9 , wherein the antimicrobial peptides are human β-defensin-2 claim 9 , β-defensin-3 claim 9 , or LL-37.14. The composition of claim 13 , wherein the compound as an active ingredient is contained at 0.001-90 wt %.15. The composition of claim 13 , wherein the composition for promoting secretion of human antimicrobial peptides in vivo is a formulation selected from the group consisting of a liquid phase claim 13 , an emulsion phase claim 13 , a suspension phase claim 13 , a cream phase claim 13 , an ointment phase claim 13 , a gel phase claim 13 , a jelly phase claim 13 , and a spray phase.16. The composition of claim 13 , wherein the composition for promoting secretion of human antimicrobial peptides in vivo is a formulation selected from the group consisting of a tablet claim 13 , a liquid claim 13 , a powder claim 13 , and an injection. This application is a continuation application of PCT International Application No. PCT/KR2010/005759 filed Aug. 27, 2010, the contents of which are incorporated herein by reference in their entirety.The following disclosure relates to a compound for promoting the secretion of human antimicrobial peptides, and more particularly, to a new compound for inducing direct or indirect expression of human β-defensin-2 and -3 and LL-37, which are human antimicrobial peptides, a method for preparing the same, and a composition comprising the same as an active ...

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25-07-2013 дата публикации

Fluorine Radiolabelling Process

Номер: US20130190529A1
Принадлежит:

The invention relates to a process for producing a process for producing an F-labelled compound, the process comprising treating a compound of formula (I) 4. A process according to wherein said rearomatisation is performed in situ.5. A process according to wherein said rearomatisation comprises the addition of a reagent which effects cleavage of Xfrom the carbon atom of the ring which is para to EDG′ in the compound of formula (IIa) claim 3 , to produce a compound of formula (II) claim 3 , wherein said reagent is an acid claim 3 , base or oxidising agent.613.-. (canceled)1517.-. (canceled)2021.-. (canceled)28. A process according to which further comprises a deprotection step comprising substituting H for said amino protecting group R claim 27 , thereby converting the group —NHRin the compound of formula (IIc″″) or (IId″″) into a —NHgroup.3233.-. (canceled)34. A process according to wherein said rearomatisation is performed in situ.35. A process according to wherein said rearomatisation comprises the addition of a reagent which effects cleavage of Xfrom the carbon atom of the ring which is para to EDG′ in the compound of formula (IIc) or formula (IId) claim 23 , wherein said reagent is an acid claim 23 , base or oxidising agent.3645.-. (canceled)47. A process according to wherein said deprotection step is performed in situ.4851.-. (canceled)52. A process according to wherein the step of treating the compound of formula (I) with [F]fluoride comprises treating the compound of formula (I) with a compound comprising F and a counter cation claim 1 , wherein the counter cation is a quaternary ammonium cation claim 1 , an alkali metal or H.5362.-. (canceled)63. A process according to wherein the oxidant is a hypervalent iodonium (III) reagent or a metal oxide.6466.-. (canceled)67. A process according to wherein the step of treating the compound of formula (I) with [F]fluoride is performed in the presence of an additive claim 1 , wherein the additive is an acid or a crown ...

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01-08-2013 дата публикации

Method for producing optically active amine compound

Номер: US20130197234A1

The present invention relates to methods for producing an optically active amine compound via a highly enantioselective hydrogenation reaction of an imine compound, wherein the imine compound is hydrogenated using a ruthenium metal complex having high catalytic activity and represented by Formula (1) RuXYAB  (1) such as RuBr 2 [(S,S)-xylskewphos][(S,S)-dpen].

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01-08-2013 дата публикации

METHOD FOR PRODUCING NITROBENZENE BY ADIABATIC NITRIDING

Номер: US20130197268A1
Принадлежит: Bayer Intellectual Property GmbH

The invention relates to a process for the continuous production of nitrobenzene by nitration of benzene with a mixture of nitric acid and sulfuric acid under adiabatic conditions, in which unreacted benzene is separated from the crude product obtained after phase separation before washing thereof, using the adiabatic heat of reaction. 19-. (canceled)10. A process for continuously producing nitrobenzene comprisinga) nitrating benzene with a mixture of nitric acid and sulfuric acid under adiabatic conditions to obtain a product;b) separating the product obtained in step a) by phase separation into an aqueous phase comprising sulfuric acid, nitrobenzene, and benzene, and an organic phase comprising nitrobenzene and benzene;c) transferring the aqueous phase obtained in step b) into an evaporator wherein the sulfuric acid is concentrated by pressure reduction, wherein a gaseous stream comprising water, nitrobenzene, and benzene is removed from the evaporator and then condensed, and wherein the resulting concentrated sulfuric acid is fed back into step a);d) separating via distillation from 20% by mass to 100% by mass of the benzene contained in the organic phase obtained in step b) by evaporating the benzene using the adiabatic heat of reaction obtained in step a), wherein a pre-purified nitrobenzene depleted of benzene is obtained;e) washing the pre-purified nitrobenzene obtained in step d) with at least one aqueous phase and subsequently separating the at least one aqueous phase from the nitrobenzene by phase separation to obtain purified nitrobenzene.11. The process of claim 10 , wherein in step d) from 20% by mass to 99.8% by mass of the benzene contained in the organic phase obtained in step b) is separated off and step e) is followed by:f) separating via distillation benzene and water from the purified nitrobenzene obtained in step e) to obtain dried pure nitrobenzene.12. The process of claim 10 , further comprising removing the water from the condensed gaseous ...

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01-08-2013 дата публикации

Method for producing bis(aminomethyl)cyclohexanes

Номер: US20130197269A1
Принадлежит: Mitsui Chemicals Inc

A method for producing bis(aminomethyl)cyclohexanes includes a nuclear hydrogenation step of producing hydrogenated phthalic acids or phthalic acid derivatives by nuclear hydrogenation of phthalic acids or phthalic acid derivatives of at least one selected from the group consisting of phthalic acids, phthalic acid esters, and phthalic acid amides; a cyanation step of treating the hydrogenated phthalic acids or phthalic acid derivatives obtained in the nuclear hydrogenation step with ammonia, thereby producing dicyanocyclohexanes; and an aminomethylation step of treating the dicyanocyclohexanes obtained in the cyanation step with hydrogen, thereby producing bis(aminomethyl)cyclohexanes. In the cyanation step, metal oxide is used as a catalyst, and the obtained dicyanocyclohexanes have a metal content of 3000 ppm or less.

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01-08-2013 дата публикации

METHOD FOR PRODUCING TRANS-1,4-BIS(AMINOMETHYL) CYCLOHEXANE

Номер: US20130197270A1
Принадлежит:

A method for producing trans-1,4-bis(aminomethyl)cyclohexane includes a nuclear hydrogenation step of producing a hydrogenated terephthalic acid or terephthalic acid derivative by nuclear hydrogenation of a terephthalic acid or terephthalic acid derivative, the terephthalic acid or terephthalic acid derivative being at least one selected from the group consisting of terephthalic acid, terephthalic acid ester, and terephthalic acid amide; a cyanation step of treating the hydrogenated terephthalic acid or terephthalic acid derivative with ammonia, thereby producing 1,4-dicyanocyclohexane, and producing trans-1,4-dicyanocyclohexane from the obtained 1,4-dicyanocyclohexane; and an aminomethylation step of treating the trans-1,4-dicyanocyclohexane with hydrogen, thereby producing trans-1,4-bis(aminomethyl)cyclohexane. 1. A method for producing trans-1 ,4-bis(aminomethyl)cyclohexane , the method comprising: 'the terephthalic acid or terephthalic acid derivative being at least one selected from the group consisting of terephthalic acid, terephthalic acid ester, and terephthalic acid amide;', 'a nuclear hydrogenation step of producing a hydrogenated terephthalic acid or terephthalic acid derivative by nuclear hydrogenation of a terephthalic acid or terephthalic acid derivative,'}a cyanation step of treating the hydrogenated terephthalic acid or terephthalic acid derivative obtained in the nuclear hydrogenation step with ammonia, thereby producing 1,4-dicyanocyclohexane, and producing trans-1,4-dicyanocyclohexane from the obtained 1,4-dicyanocyclohexane; andan aminomethylation step of treating the trans-1,4-dicyanocyclohexane obtained in the cyanation step with hydrogen, thereby producing trans-1,4-bis(aminomethyl)cyclohexane,wherein metal oxide is used as a catalyst in the cyanation step, and the obtained trans-1,4-dicyanocyclohexane has a metal content of 3000 ppm or less.2. A method for producing trans-1 ,4-bis(aminomethyl)cyclohexane , the method comprising:a cyanation ...

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08-08-2013 дата публикации

PROCESS FOR PRODUCING COMPOUNDS COMPRISING NITRILE FUNCTIONS

Номер: US20130204001A1
Принадлежит: Rhodia Operations

The production of compounds comprising nitrile functions and of cyclic imide compounds is described. Further described, is the production of compounds comprising nitrile functions from compounds comprising carboxylic functions, optionally of natural and renewable origin, and from a mixture N of dinitriles comprising 2-methylglutaronitrile (MGN), 2-ethylsuccinonitrile (ESN) and adiponitrile (AdN). 1. A process for preparing at least one nitrile of general formula I{'br': None, 'sub': v', '1', 'w, '(NC)—R—(CN)\u2003\u2003(I)'} {'br': None, 'sub': x', '1', 'y, '(HOOC)—R—(COOH)\u2003\u2003(II)'}, 'and at least cyclic imides 3-methylglutarimide and 3-ethylsuccinimide, by reacting at least one carboxylic acid of general formula II'}and a mixture N of dinitriles comprising 2-methylglutaronitrile (MGN), 2-ethylsuccinonitrile (ESN) and adiponitrile (AdN),whereinx, y are equal to 0 or 1 with (x+y) equal to 1 or 2,v, w are equal to 0 or 1 with (v+w) equal to 1 or 2, and from 4 carbon atoms to 34 carbon atoms when (x+y) is equal to 2, and', 'from 2 carbon atoms to 22 carbon atoms when (x+y) is equal to 1., 'R1 represents a linear or branched, saturated or unsaturated hydrocarbon-based group which can comprise heteroatoms, comprising2. The process as defined in claim 1 , wherein the mixture N of dinitriles is a mixture resulting from the process for producing adiponitrile by double hydrocyanation of butadiene.3. The process as defined in claim 1 , wherein the mixture N of dinitriles has the following composition by weight:2-Methylglutaronitrile from 70% to 95%,2-Ethylsuccinonitrile from 5% to 30%, andAdiponitrile from 0% to 10%, andwherein the remaining portion of the composition is composed of various impurities.4. The process as defined in claim 1 , wherein the compound of formula II is derived from a renewable matter of vegetable or animal origin.5. The process as defined in claim 4 , wherein the compound of formula II is selected from the group consisting of a caproic acid ...

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08-08-2013 дата публикации

NEW PROCESS FOR THE RESOLUTION OF ENANTIOMERS OF (3,4 DIMETHOXY-BICYCLO[4.2.0]OCTA-1,3,5-TRIEN-7-YL)NITRILE AND APPLICATION IN THE SYNTHESIS OF IVABRADINE

Номер: US20130204032A1
Принадлежит: LES LABORATOIRES SERVIER

Process for the optical resolution of the compound of formula (I): 4. The process of claim 3 , wherein the reduction of the compound of formula (Ia) is carried out in the presence of palladium-on-carbon and HCl under a hydrogen atmosphere or in the presence of sodium tetraborohydride and trifluoroacetic acid. The present invention relates to a process for the optical resolution of (3,4-dimethoxy-bicyclo[4.2.0]octa-1,3,5-trien-7-yl)nitrile of formula (I) and to the application thereof in the synthesis of ivabradine, of its addition salts with a pharmaceutically acceptable acid and of their hydrates.Ivabradine of formula (II):or 3-{3-[{[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}(methyl)amino]-propyl}-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one, and its addition salts with a pharmaceutically acceptable acid, and more especially its hydrochloride, have very valuable pharmacological and therapeutic properties, especially bradycardic properties, making these compounds useful in the treatment or prevention of various clinical situations of myocardial ischaemia such as angina pectoris, myocardial infarct and associated rhythm disturbances, and also in various pathologies involving rhythm disturbances, especially supraventricular rhythm disturbances, and in heart failure.The preparation and therapeutic use of ivabradine and its addition salts with a pharmaceutically acceptable acid, and more especially its hydrochloride, have been described in the European patent specification EP 0 534 859.That patent specification describes the synthesis of ivabradine starting from the compound of formula (III):The compound of formula (III) is prepared starting from the compound of formula (IV):by resolution using camphorsulphonic acid.The compound of formula (III) is an important intermediate in the synthesis of ivabradine.Resolution of the secondary amine of formula (IV) results in the compound of formula (III) in only a low yield (4 to 5%).However, in view ...

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08-08-2013 дата публикации

DECOLORIZATION OF AMINES

Номер: US20130204044A1
Принадлежит:

The present invention provides methods that are used to decolorize compositions containing one or more amines in the presence of one or more weak acids. Significantly, the weak acids, particularly organic acids such as glacial acetic acid, when used in combination with a heat treatment produce dramatically less by-products than do the stronger mineral acids, making heat treatments and subsequent separation techniques more effective while producing less waste. In some modes of practice, the weak acids do not need to be neutralized, eliminating neutralizing steps and waste streams associated with neutralization. Low color products can be obtained easily at very high yield as a consequence. 1. A method of reducing color of a composition including one or more amines and one or more color bodies , comprising the steps of:(a) providing the composition, wherein the composition has an initial color;(b) heat treating the composition in the presence of at least one weak acid under conditions effective to modify the composition so that a separation technique can more effectively separate at least a portion of the amines from at least a portion of the color bodies; and(c) after heat treating, using at least the separation technique to recover at least a portion of the amines from the heat treated composition in a manner such that the recovered portion has less color relative to the initial color.2. The method of claim 1 , further comprising the step of using a color characteristic of the heat treated composition to help determine when heat treating is complete.3. The method of claim 1 , wherein step (a) comprises providing a amine composition having a color in the range from about 400 APHA to about 5000 APHA.4. The method of claim 1 , wherein the amine composition comprises linear triethylenetetramine and/or a congener thereof.5. The method of claim claim 1 , wherein the at least one weak acid comprises an organic acid.6. The method of claim 1 , wherein the at least one weak ...

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15-08-2013 дата публикации

New process for the resolution of enantiomers of (3,4 dimethoxy-bicyclo[4.2.0]octa-1,3,5-trien-7-yl)nitrile and application in the synthesis of ivabradine

Номер: US20130211070A1
Принадлежит: Laboratoires Servier SAS

Process for the optical resolution of the compound of formula (I): by chiral chromatography. Application in the synthesis of ivabradine, of its addition salts with a pharmaceutically acceptable acid and of their hydrates.

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15-08-2013 дата публикации

Process for Preparing Esteramide Compounds

Номер: US20130211129A1
Принадлежит: Rhodia Operations

The present invention concerns a process for preparing esteramide compounds. More particularly, the invention relates to a process for preparing esteramide compounds by reaction between a diester and an amine, in the presence of a basic compound, wherein the basic compound and the amine in gaseous form are co-added to the diester, the reaction being conducted at a temperature of 30° C. or higher.

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15-08-2013 дата публикации

MONITORING OF THE STOICHIOMETRIC RATIO IN THE REACTION OF NITROAROMATICS WITH HYDROGEN

Номер: US20130211141A1
Принадлежит:

The present invention relates to a continuous process for preparing at least one aromatic amine by hydrogenation of at least one nitroaromatic by means of hydrogen, where a liquid phase comprising at least the aromatic amine and a gas phase comprising at least hydrogen are present, in the presence of a catalyst suspended in the liquid phase at a temperature of from 50 to 250° C. and a pressure of from 5 to 50 bar, wherein the pressure in the reactor is kept essentially constant by continuous adaptation of the amount of hydrogen fed to the reactor, the total amount of hydrogen fed to the reactor is monitored and the introduction of the at least one nitroaromatic is interrupted if the hydrogen uptake in the reactor is not at least 50 mol % of the amount of hydrogen required for stoichiometric reaction of the at least one nitroaromatic to form the at least one aromatic amine. 1. A continuous process for preparing at least one aromatic amine by hydrogenation of at least one nitroaromatic by means of hydrogen , where a liquid phase comprising at least the aromatic amine and a gas phase comprising at least hydrogen are present , in the presence of a catalyst suspended in the liquid phase at a temperature of from 50 to 250° C. and a pressure of from 5 to 50 bar , whereinthe pressure in the reactor is kept essentially constant by continuous adaptation of the amount of hydrogen fed to the reactor,the total amount of hydrogen fed to the reactor is monitored andthe introduction of the at least one nitroaromatic is interrupted if the hydrogen uptake in the reactor is not at least 50 mol %, preferably at least 70 mol %, particularly preferably at least 90 mol %, very particularly preferably at least 95 mol %, in particular at least 98 mol %, of the amount of hydrogen required for stoichiometric reaction of the at least one nitroaromatic to form the at least one aromatic amine.2. The process according to claim 1 , wherein the hydrogen uptake in the reactor corresponding to the ...

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15-08-2013 дата публикации

HALOGENATED DIETHYLTOLUENEDIAMINES

Номер: US20130211142A1
Принадлежит: Lonza Ltd.

Disclosed are halogenated diethyltoluenediamines of formula

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22-08-2013 дата публикации

ELECTRODE AND ELECTRODE COATING

Номер: US20130213799A1
Принадлежит: BAYER MATERIALSCIENCE AG

The invention describes an electrode and an electrode coating which are based on a catalyst containing finely divided carbon modifications and noble metal (oxide)s. 1. A catalyst for preparing chlorine by means of electrolysis of electrolytes comprising chlorine ions , wherein said catalyst comprises at least one noble metal of transition group VIIIa (Fe , Ru , Rh , Pd , Os , Ir , Pt) of the Periodic Table of the Elements and/or an oxide of these noble metals , wherein said catalyst additionally comprises at least one finely divided carbon modification selected from the group consisting of diamond , doped diamond , fullerene , carbon nanotubes , and vitreous carbon , and wherein said catalyst optionally comprises at least one valve metal and/or valve metal oxide.2. The catalyst of claim 1 , wherein said catalyst comprises from 10 to 90 mol % of said at least one finely divided carbon modification and from 0.05 to 40 mol % of said at least one noble metal and/or noble metal oxide.3. The catalyst of claim 2 , wherein said catalyst comprises from 20 to 80 mol % of said at least one finely divided carbon modification and from 1 to 20 mol % of said at least one noble metal and/or noble metal oxide.4. The catalyst of claim 1 , wherein said catalyst comprises from 0.05 to 40 mol % of said at least one noble metal and/or noble metal oxide claim 1 , from 9.95 to 60 mol % of said at least one valve metal and/or valve metal oxide claim 1 , and from 20 to 90 mol % of said at least one finely divided carbon modification.5. The catalyst of claim 1 , wherein said at least one finely divided carbon modification is diamond and/or boron-doped diamond.6. The catalyst of claim 1 , wherein said at least one noble metal and/or noble metal oxide is selected from the group consisting of iridium claim 1 , ruthenium claim 1 , rhodium claim 1 , palladium claim 1 , platinum claim 1 , and oxides thereof.7. The catalyst of claim 1 , wherein said at least one valve metal and/or valve metal oxide ...

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22-08-2013 дата публикации

SYNTHESIS OF CYCLOHEXANE DERIVATIVES USEFUL AS SENSATES IN CONSUMER PRODUCTS

Номер: US20130216486A1
Принадлежит: The Procter & Gamble Company

The present invention provides synthetic routes for preparing various isomers of cyclohexane-based coolants, such as menthyl esters and menthanecarboxamide derivatives, in particular those substituted at the amide nitrogen, for example with an aromatic ring or aryl moiety. Such structures have high cooling potency and long lasting sensory effect, which make them useful in a wide variety of consumer products. One synthetic route involves a copper catalyzed coupling of a primary menthanecarboxamide with an aryl halide, such reaction working best in the presence of potassium phosphate and water. Using this synthetic route, specific isomers can be prepared including the menthanecarboxamide isomer having the same configuration as l-menthol and new isomers such as a neoisomer having opposite stereochemistry at the carboxamide (C-1) position. The neoisomer unexpectedly has potent and long lasting cooling effect. Preparation schemes for neoisomers of other menthyl derivatives which are useful as coolants, including esters, ethers, carboxy esters and other N-substituted carboxamides are also provided. 2. The process of wherein the reaction is conducted in the presence of potassium phosphate and the copper catalyst is a copper halide.3. The process of wherein the copper halide is copper (I) iodide.4. The process of wherein the primary menthane carboxamide is prepared by reacting a menthane acid chloride with ammonia under aqueous conditions.5. The process of wherein the menthane carboxamide is prepared by hydrolysis of a corresponding menthane nitrile.6. The process of wherein the stereochemistry of the starting menthane carboxamide is maintained through the coupling reaction with aryl halide to produce the N-substituted menthane carboxamide.7. The process of wherein (1S claim 6 ,2S claim 6 ,5R)-menthane carboxamide is reacted with aryl halide to produce neoisomers having 1S claim 6 ,2S claim 6 ,5R configuration of N-aryl substituted menthane carboxamide.8. A process for ...

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22-08-2013 дата публикации

Process for the preparation of substituted n-(benzyl)cyclopropanamines by imine hydrogenation

Номер: US20130217910A1
Принадлежит: Bayer Intellectual Property GmbH

The present invention relates to a process for the preparation of substituted N-(benzyl)cyclopropanamines of the general formula (II) starting from N-[(aryl)methylene]cyclopropanamine derivatives. The present invention further provides the N-[(arypmethylene]cyclopropanamine derivatives used as starting compounds in this process according to the invention, and their use for the preparation of substituted N (benzyl)cyclopropanamines.

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22-08-2013 дата публикации

METHOD FOR PRODUCTION OF F-18 LABELED AMYLOID BETA LIGANDS

Номер: US20130217920A1
Принадлежит: PIRAMAL IMAGING SA

This invention relates to methods, which provide access to [F-18]fluoropegylated (aryl/heteraryl vinyl)-phenyl methyl amine derivatives. 2. A method according to claim 1 , wherein PG is selected from the group consisting of:a) Boc,b) Trityl andc) 4-Methoxytrityl.3. A method according to claim 1 , wherein LG is selected from the group consisting of:a) Halogen andb) Sulfonyloxy,Halogen is chloro, bromo or iodo.4. A method according to claim 3 , wherein Sulfonyloxy is selected from the group comprising:a) Methanesulfonyloxy,b) p-Toluenesulfonyloxy,c) (4-Nitrophenyl)sulfonyloxy,d) (4-Bromophenyl)sulfonyloxy.5. A method according to claim 1 , wherein n=3 and X=CH.6. A method according to claim 1 , wherein n=3 claim 1 , X=CH claim 1 , R=Boc claim 1 , and LG=Methanesulfonyloxy.7. A method according to claim 1 , wherein 10-50 μmol of a compound of formula II is used.8. A method according to claim 7 , wherein 10-30 μmol of a compound of formula II is used.9. A method according to claim 1 , wherein 10 or more μmol of a compound of formula II is used.10. A method according to claim 1 , wherein the method is performed as a fully automated process. This invention relates to methods, which provide access to [F-18]fluoropegylated (aryl/heteraryl vinyl)-phenyl methyl amine derivatives.Alzheimer's Disease (AD) is a progressive neurodegenerative disorder marked by loss of memory, cognition, and behavioral stability. AD is defined pathologically by extracellular senile plaques comprised of fibrillar deposits of the beta-amyloid peptide (Aβ) and neurofibrillary tangles comprised of paired helical filaments of hyperphosphorylated tau. The 39-43 amino acids comprising Aβ peptides are derived from the larger amyloid precursor protein (APP). In the amyloidogenic pathway, Aβ peptides are cleaved from APP by the sequential proteolysis by beta- and gamma-secretases. Aβ peptides are released as soluble proteins and are detected at low level in the cerebrospinal fluid (CSF) in normal aging ...

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29-08-2013 дата публикации

USE OF NITROANILINE DERIVATIVES FOR THE PRODUCTION OF NITRIC OXIDE

Номер: US20130224083A1
Принадлежит: STMicroelectronics S.r.I.

The present invention relates to the use of a nitroaniline derivative of Formula I for the production of nitric oxide and for the preparation of a medicament for the treatment of a disease wherein the administration of nitric oxide is beneficial. The present invention furthermore relates to a method for the production of NO irradiating a nitroaniline derivative of Formula I, a kit comprising a nitroaniline derivative of Formula I and a carrier and to a system comprising a source of radiations and a container associated to a nitroaniline derivative of Formula I. In Formula I, R and Rare each independently hydrogen or a C-Calkyl group; Ris hydrogen or an alkyl group. 2. The kit according to claim 1 , wherein:{'sup': II', 'III', 'IV', 'V', 'VI, 'sub': 2', '18', '2', '3', '3', '3, 'Ris Ak-Y, wherein Ak is a branched or unbranched C-Calkyl group optionally substituted with —OH or NH, and Y is a tail-group selected from the group consisting of hydrogen, halogen, —SH, —S—SR, —Si(OR), —Si—X, and —CH═CRR;'}{'sup': 'III', 'Ris selected from the group consisting of alkyl group, aryl group, aralkyl group, alkenyl group, alkynyl group and heterocyclic group;'}{'sup': 'III', 'Ris an alkyl group;'}{'sup': V', 'VI, 'Rand Rare independently hydrogen or alkyl group; and'}X is halogen.3. The kit according to claim 1 , wherein said nitroaniline derivative of Formula (I) is 4-nitro-3-(trifluoromethyl)aniline.4. The kit according to claim 1 , wherein said carrier has a minor molar absorptivity in the wavelength comprised between 300 and 500 nm.5. The kit according to claim 1 , wherein said carrier is a liquid solution.6. The kit according to claim 1 , wherein said carrier is a solid substrate selected from the group consisting of a metal; an inorganic oxide; and a plastic polymeric material.7. The kit according to claim 6 , wherein said nitroaniline derivative of Formula (I) is chemically bound to said solid substrate without forming an amide bond.8. The kit according to claim 7 , ...

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29-08-2013 дата публикации

METHOD FOR PREPARING ALISKIREN AND ITS INTERMEDIATES THEREOF

Номер: US20130225841A1

A method for preparing Aliskiren and intermediate thereof, which comprises the following steps: reacting 4-bromo-1-methoxy-2-(3-methoxypropoxy)benzene with magnesium isopropyl chloride and n-BuLi to obtain the compound of formula XXII; reacting the product of methylsulfonylation of the compound of formula XIX with anhydrous LiBr to obtain the compound of formula XXI; obtaining the intermediate of Aliskiren shown as formula XV by reacting the compound of formula XXII with the compound of formula XXI in an ether as the solvent and in the presence of a catalyst containing iron; then reacting the compound of formula XV with the compound of formula VII to obtain the compound of formula XXIII, following removing Rfrom the amino group and obtaining Aliskiren shown as formula I. 2. The method according to wherein the ether class solvent in step (1) is one selected from diethyl ether claim 1 , tetrahydrofuran or 1 claim 1 ,2-dimethoxyethane.3. The method according to wherein the inert solvent in step (2) is methylene chloride or tetrahydrofuran.4. The method according to wherein the ketone class solvent in step (3) is acetone or 2-butanone; and the molar ratio between lithium bromide and the compound of formula XX is 1.1 to 5.5. The method according to wherein the said ether class solvent in step (4) is either one or mixture of any two selected from diethyl ether claim 1 , tetrahydrofuran or 1 claim 1 ,2-dimethoxyethane; the said iron-contained catalyst is selected from iron(III) acetylacetonate or Iron(III) chloride; and the reaction temperature is −15° C.˜20° C.7. The method according to for preparing the Aliskiren compound of formula I claim 6 , wherein the reaction in step (a) between the compound of formula XV and the compound of formula VII to obtain the compound of formula XXIII is implemented in an inert solvent.8. The method according to for preparing the Aliskiren compound of formula I claim 7 , wherein the inert solvent is one selected from dioxane or toluene.9. ...

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29-08-2013 дата публикации

TRANSAMINATION OF NITROGEN-CONTAINING COMPOUNDS TO HIGH MOLECULAR WEIGHT POLYALKYLENEAMINES

Номер: US20130225864A1
Автор: King Stephen W.
Принадлежит:

A process for preparing high molecular weight acyclic polyamines comprising providing a reaction mixture that includes at least a first component comprising a first organic, nitrogen-containing compound that contains at least two non-tertiary amine groups separated from one another by a ternary or higher carbon atom spacing that can be transaminated in the presence of a hydrogenation/dehydrogenation catalyst to form a mixture of higher molecular weight, acyclic polyamines while minimizing the formation of cyclic polyamines. 1. A method of making a linear high molecular weight polyamine-containing product mixture comprising the steps of:(a) providing a reaction composition comprising one or more nitrogen-containing compounds comprising a first component that has at least two non-tertiary amine groups separated from one another by at least a ternary or higher carbon atom spacing (C3 or greater spacing) and, optionally, a second component that has at least two nitrogen containing groups separated from one another by a second carbon atom spacing; and(b) subjecting the reaction composition to a transamination reaction in the presence of a hydrogenation/dehydrogenation catalyst to obtain the linear high molecular weight polyamine-containing mixture.2. The method of claim 1 , wherein the component comprises a nitrogen-containing compound having (i) at least two non-tertiary amine groups separated from one another by a ternary or greater carbon atom spacing (C3 or greater spacing) claim 1 , (ii) at least two nitrile functionalities separated by at least one carbon atom (C1 spacing) claim 1 , (iii) at least one nitrile functionality and one non-tertiary amine functionality separated from one another by a binary or greater carbon atom spacing (C2 or greater spacing).6. The method of claim 3 , wherein each R is H.7. A method of making a mixture of congeners of high molecular weight polyamines claim 3 , comprising the steps of: providing a reaction mixture comprising first ...

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05-09-2013 дата публикации

PROCESS FOR PREPARING 1,6-HEXANEDIOL

Номер: US20130231505A1
Принадлежит: E I DU PONT DE NEMOURS AND COMPANY

Disclosed are processes for preparing 1,6-hexanediol from levoglucosenone. In one embodiment, the process comprises contacting levoglucosenone with hydrogen in the presence of a hydrogenation catalyst comprising palladium, platinum/tungsten, nickel/tungsten, rhodium/rhenium, or mixtures thereof at a first temperature between about 50° C. and 100° C. and at a first reaction pressure between about 50 psi and 2000 psi for a first reaction period, and at a second temperature between about 120° C. and 250° C. and at a second pressure between about 500 psi and 2000 psi for a second reaction period to form a product mixture comprising 1,6-hexanediol, wherein the first reaction period is the amount of time in which the levoglucosenone has a conversion of at least about 95%. In one embodiment, the 1,6-hexanediol is converted to 1,6-diaminohexane. 1. A process comprising:(a) contacting levoglucosenone with hydrogen in the presence of a hydrogenation catalyst comprising palladium, platinum/tungsten, nickel/tungsten, rhodium/rhenium, or mixtures thereof at a first temperature between about 50° C. and 100° C. and at a first reaction pressure between about 50 psi and 2000 psi for a first reaction period, wherein the first reaction period is the amount of time in which the levoglucosenone has a conversion of at least about 95%; and at a second temperature between about 120° C. and 250° C. and at a second reaction pressure between about 500 psi and 2000 psi for a second reaction period to form a final product mixture comprising 1,6-hexanediol;(b) isolating the 1,6-hexanediol from the final product mixture;(c) contacting the 1,6-hexanediol with ammonia and hydrogen in the presence of a reductive amination catalyst at a temperature and for a time sufficient to form an amination product mixture comprising 1,6-diaminohexane; and(d) optionally, isolating the 1,6-diaminohexane from the amination product mixture.2. The process of claim 1 , wherein the hydrogenation catalyst further ...

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12-09-2013 дата публикации

Process for preparing amino hydrocarbons by direct amination of hydrocarbons

Номер: US20130233721A1
Принадлежит: BASF SE

The present invention relates to a process for direct amination of hydrocarbons to amino hydrocarbons, comprising (a) the reaction of a reactant stream E comprising at least one hydrocarbon and at least one aminating reagent to give a reaction mixture R comprising at least one amino hydrocarbon and hydrogen in a reaction zone RZ, and (b) electrochemical removal of at least a portion of the hydrogen formed in the reaction from the reaction mixture R by means of at least one gas-tight membrane electrode assembly which is in contact with the reaction zone RZ on the retentate side and which has at least one selectively proton-conducting membrane, at least a portion of the hydrogen being oxidized over an anode catalyst to protons on the retentate side of the membrane, and the protons, after passing through the membrane, being partly or fully reduced by applying a voltage over a cathode catalyst to give hydrogen on the permeate side.

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12-09-2013 дата публикации

PROCESS FOR PREPARING AMINO HYDROCARBONS BY DIRECT AMINATION OF HYDROCARBONS

Номер: US20130236801A1
Принадлежит: BASF SE

The present invention relates to a process for direct amination of hydrocarbons to amino hydrocarbons, comprising 1. A process for direct amination of hydrocarbons to amino hydrocarbons , comprising(a) the reaction of a reactant stream E comprising at least one hydrocarbon and at least one aminating reagent to give a reaction mixture R comprising at least one amino hydrocarbon and hydrogen in a reaction zone RZ, and(b) electrochemical removal of at least a portion of the hydrogen formed in the reaction from the reaction mixture R by means of at least one gas-tight membrane electrode assembly which is in contact with the reaction zone RZ on the retentate side and which has at least one selectively proton-conducting membrane,at least a portion of the hydrogen being oxidized over an anode catalyst to protons on the retentate side of the membrane, and the protons, after passing through the membrane, being partly or fully reacted with an oxidizing agent over a cathode catalyst to give water on the permeate side, and the oxidizing agent originating from a stream O which is contacted with the permeate side of the membrane.2. The process according to claim 1 , wherein the oxidizing agent is oxygen.3. The process according to or claim 1 , wherein the hydrogen is removed from the reaction zone RZ.4. The process according to one or more of to claim 1 , wherein the electrode catalyst present on the retentate side serves simultaneously as an amination catalyst for the conversion of the hydrocarbons to amino hydrocarbons.5. The process according to one or more of to claim 1 , wherein a gas distributor layer present on the retentate side has been functionalized with an amination catalyst.6. The process according to one or more of to claim 1 , wherein the electrodes of the membrane electrode assembly (MEA) comprising an amination catalyst serve for the conversion of the hydrocarbons to amino hydrocarbons.7. The process according to one or more of to claim 1 , wherein claim 1 , in ...

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12-09-2013 дата публикации

AMINES HAVING SECONDARY ALIPHATIC AMINO GROUPS

Номер: US20130237681A1
Автор: BURCKHARDT Urs
Принадлежит: SIKA TECHNOLOGY AG

The present invention relates to novel amides having secondary amino groups, a process for preparing them, adducts of these amines and their uses. The amides can be prepared in a simple way from readily available starting materials. They and their adducts have, in particular, a low viscosity and are suitable as constituent of polyurethane and polyurea compositions having excellent processability and high flexibility, and also as constituent of epoxy resin compositions, in particular coatings. 2. The amine of formula (I) according to claim 1 , wherein Rand Reach stand for a methyl radical and/or Rstands for a hydrogen atom.3. The amine of formula (I) according to claim 1 , wherein Rstands for a hydrogen atom or for a hydrocarbon radical with 1 to 12 carbon atoms claim 1 , optionally containing an ether oxygen.4. The amine of formula (I) according to claim 1 , wherein Rstands for a hydrogen atom or a linear or branched alkyl radical with 1 to 11 carbon atoms claim 1 , optionally with cyclic fractions and optionally with at least one heteroatom or for a mono- or polyunsaturated linear or branched hydrocarbon radical with 5 to 11 carbon atoms or for an optionally substituted aromatic or heteroaromatic six-membered ring.5. The amine of formula (I) according to claim 1 , wherein Xstands for a phenyl claim 1 , biphenyl or naphthyl radical claim 1 , where this radical is optionally substituted claim 1 , with linear or branched alkyl radicals with 1 to 6 carbon atoms claim 1 , with alkoxy groups with 1 to 6 carbon atoms claim 1 , with ester groups with 1 to 6 carbon atoms or with nitrilo groups.7. The method of synthesis of an amine of formula (I) according to claim 6 , wherein the process is carried out in such a way that at one amine PA of formula (II) is condensed with at least one aldehyde ALD of formula (III) to form an aldimine which is then hydrogenated.8. The method according to claim 6 , wherein the amine PA of formula (II) is selected from the group consisting of 1 ...

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19-09-2013 дата публикации

HCl Polymorphs of 3-((2-(Dimethylamino)methyl(cyclohex-1-yl))phenol

Номер: US20130245125A1
Принадлежит: GRUENENTHAL GmbH

A crystalline salt of 3-[2-(dimethylamino)methyl(cyclohex-1-yl)] phenol and hydrogen chloride, preferably in a 1:1 composition, including various crystalline forms of this salt, processes for preparing the various crystalline forms of this salt, pharmaceutical compositions containing the various crystalline forms of this salt, and the use of this salt as a pharmacologically active agent in a pharmaceutical composition to treat or inhibit pain or other disorders or disease states. 1. A crystalline salt of hydrogen chloride and 3-[2-(dimethylamino)methyl-(cyclohex-1-yl)]phenol.3. A crystalline salt according to claim 1 , wherein said salt is in the form of a diastereomer or a mixture of enantiomeric diastereomers wherein the phenol ring and the dimethylaminomethyl group are in a trans configuration.4. A crystalline salt according to claim 3 , wherein said salt is in the form of an enantiomer with a (1R claim 3 ,2R) absolute configuration.5. A crystalline salt according to claim 1 , wherein said salt exhibits a characteristic X-ray diffraction pattern within the range from 2° to 35° 2θ with characteristic lines corresponding to the following 2theta values: 11.2 (w) claim 1 , 14.1 (m) claim 1 , 17.1 (w) claim 1 , 19.5 (w) claim 1 , 19.8 (vs) claim 1 , 20.5 (w) claim 1 , 21.5 (m) claim 1 , 24.1 (m) claim 1 , 26.1 (s) claim 1 , 26.8 (w) claim 1 , and 31.3 (m).6. A crystalline salt according to claim 1 , which exhibits the X-ray diffraction pattern of .7. A crystalline salt according to claim 1 , which exhibits the Raman spectrum of .8. A crystalline salt according to claim 1 , wherein said salt is crystalline form III and exhibits a characteristic X-ray diffraction pattern within the range from 2° to 35° 2θ with pronounced characteristic lines corresponding to the following 2theta values: 6.9 (s) claim 1 , 13.9 (m) claim 1 , 16.3 (m) claim 1 , 17.7 (w) claim 1 , 20.9 (vs) claim 1 , 22.1 (w) claim 1 , 22.5 (w) claim 1 , and 27.8 (w).9. A crystalline salt according to claim ...

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19-09-2013 дата публикации

Process For Making Amides

Номер: US20130245297A1
Принадлежит: BASF SE

Provided are processes for making an amide of a carboxylic acid by reacting an amine of the formula (I) 2. The process of claim 1 , wherein measures (a) and (b) are carried out without the use of any organic solvent.3. The process of claim 1 , wherein the reaction in measure (a) is carried out at a temperature in the range of from 130 to 230° C.4. The process of claim 1 , wherein the carboxylic acid comprises lactic acid.5. The process of claim 1 , wherein the amine according to formula (I) comprises methylamine claim 1 , dimethylamine claim 1 , ethylamine claim 1 , diethylamine claim 1 , n-propylamine claim 1 , isopropylamine claim 1 , diisopropylamine claim 1 , n-butylamine claim 1 , iso-butylamine claim 1 , tert-butylamine claim 1 , methyl n-propylamine claim 1 , n-methyl-n-ethyl amine claim 1 , or methyl iso-propylamine.6. The process of claim 1 , wherein the single reactor is connected to a fractionation column and a condenser.7. The process of claim 1 , wherein the single reactor is connected to a combination of two fractionation columns and two condensers.8. The process of claim 1 , wherein the step for re-introducing the unreacted amine according to formula (I) into the reaction mixture comprises using liquid jet nozzles.9. The process of claim 1 , wherein the carboxylic acid comprises caprylic acid claim 1 , capric acid claim 1 , or lauric acid and the amine comprises dimethylamine or diethylamine.10. The process of claim 1 , wherein the molar ratio of amine according to formula (I) to carboxylic acid is in the range of from 1.2:1 to 1:1 This application claims the benefit under 35 U.S.C. §119(e) to U.S. Provisional Application No. 61/612,452, filed Mar. 19, 2012, which is incorporated herein by reference in its entirety.The present invention is directed towards a process for making an amide of a carboxylic acid by reacting an amine of the formula (I)H—NRR  (I)Rand Rbeing defined as being the same or different,Rbeing selected from C-C-alkyl,Rbeing selected ...

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19-09-2013 дата публикации

PROCESS FOR THE PRODUCTION OF ALIPHATIC ISOCYANATES

Номер: US20130245314A1
Принадлежит: Dow Global Technologies LLC

The present invention is an aliphatic or cycloaliphatic isocyanate obtained form a process comprising the steps of reacting an aliphatic or cycloaliphatic primary amine, with phosgene in the presence of an inert solvent, wherein the initial reaction temperature is between 100 and 130° C. and the temperature is subsequently ramped to 150 to 180° C. during the course of the reaction, the solvent to amine weight ratio is 95:5 to 80:20, the total reaction pressure is maintained between 50 and 350 psig and the amine is rapidly dispersed in the phosgene through injection in a region of high efficiency mixing. 1. An aliphatic or cycloaliphatic isocyanate obtained from a process comprising:reacting an aliphatic or cycloaliphatic primary amine, or the hydrochloride or carbonate salt thereof, with phosgene in the presence of an inert solvent wherein the initial reaction temperature is between 100 and 130° C. and within 60 minutes of reaching said reaction temperature,subsequently increasing the temperature to 150 to 180° C. during the course of the reaction over a time span of about 10 minutes or less,maintaining the solvent to amine weight ratio from 95:5 to 80:20,maintaining the total reaction pressure between 50 and 350 psig anddispersing the amine in the phosgene.2. The aliphatic or cycloaliphatic isocyanate of wherein the amine is dispersed in the phosgene through injection.3. The process of claim 1 , wherein phosgene is used as a co-solvent.4. An aliphatic or cycloaliphatic isocyanate obtained from process comprising:reacting an aliphatic or cycloaliphatic amine, or the hydrochloride or carbonate salt thereof, with phosgene in the presence of an inert solvent wherein the reaction is done in two or more sequential reactors,maintaining reactor temperature from 100 to 130° C.,controlling the solvent to amine weight ration is 95:5 to 80:20, and the total reactor pressure from 50 to 350 psig andproviding a residence time in the first reactor of less than 5 minutes; ...

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26-09-2013 дата публикации

METHOD FOR PRODUCING CYANOACETIC ACID, METHOD FOR PRODUCING CYANOACETIC ACID DERIVATIVE AND METHOD FOR PRODUCING METAL CONTAINING COMPOUND

Номер: US20130253213A1

Provided is a method for producing cyanoacetic acid in a hydrolysis reaction of a predetermined cyanoacetate in the presence of an acid catalyst. Further, are provided methods for producing a cyanoacetic acid derivative and a metal containing compound by using the produced cyanoacetic acid as a staring material. Herein, the method for producing cyanoacetic acid enables the content of a malonic acid byproduct generated in the hydrolysis reaction to be greatly lowered, allowing the produced cyanoacetic acid to be used as a starting material without any purification treatments. Those advantageous effects result in the great improvement in the purity and yields of the cyanoacetic acid derivative and the metal containing compound produced by said cyanoacetic acid. Accordingly, the above mentioned methods make it possible to produce cyanoacetic acid, the cyanoacetic acid derivative and the metal containing compound, as excellent in the productivity and economical efficiency. 2. The method for producing cyanoacetic acid according to claim 1 , the alcohol produced in the hydrolysis reaction is included in 0.5 to 20 mol % with respect to the produced cyanoacetic acid claim 1 , when hydrolysis reaction is completed.3. The method for producing cyanoacetic acid according to claim 1 , the cyanoacetate of the formula (1) is included in 0.5 to 2.0 mol % with respect to the produced cyanoacetic acid claim 1 , when the hydrolysis reaction is completed.4. The method for producing cyanoacetic acid according to claim 1 , wherein the acid catalyst is selected from a group of sulfuric acid claim 1 , hydrochloric acid claim 1 , acetic acid claim 1 , cyanoacetic acid claim 1 , phosphoric acid claim 1 , and p-toluenesulfonic acid.5. The method for producing cyanoacetic acid according to claim 1 , wherein the acid catalyst is used in 0.2 to 10 mol % with respect to the cyanoacetate of the formula (1) in the hydrolysis reaction.6. The method for producing cyanoacetic acid according to claim 5 ...

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26-09-2013 дата публикации

PROCESS FOR THE PRODUCTION OF AMIDES

Номер: US20130253225A1
Принадлежит:

The present invention relates to a process for the preparation of compounds of formula I 2. A compound of formula IV according to claim 1 , wherein Rand Rare methyl.4. A compound of formula IV prepared by the process of . This application is a divisional application of U.S. Ser. No. 13/198,739 filed Jan. 8, 2013, which is a divisional application of U.S. Ser. No. 12/066,683 filed Jul. 16, 2008, which is a 371 of International Application No. PCT/EP2006/008982 filed Sep. 14, 2006, which claims priority to CH 01520/05 filed Sep. 16, 2005 and CH 0296/06 filed Feb. 24, 2006, the contents of which are incorporated herein by reference.The present invention relates to a process for the preparation of pyrazolyl-4-carboxylic acid benzo-norbornen-5-yl-amides and also to novel intermediates for use in such a process. The present invention further relates to a novel crystal modification of syn-3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid (9-isopropyl-1,2,3,4-tetrahydro-1,4-methano-naphthalen-5-yl)-amide, compositions comprising it and to the use thereof in the control of fungus infestation in cultivated plants.Pyrazolyl-4-carboxylic acid benzonorbornen-5-yl-amides, for example 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid (9-isopropyl-1,2,3,4-tetrahydro-1,4-methano-naphthalen-5-yl)-amide, are valuable fungicides, such as are described, for example, in WO 04/035589.WO 04/035589 describes a process for the preparation of pyrazolyl-4-carboxylic acid benzonorbornen-5-yl-amides (see Scheme 1):According to WO 04/035589, a 3-nitro-dehydrobenzene generated, for example, from 6-nitro-anthralinic acids of formula (A) wherein Rand Rmay be, inter alia, hydrogen, is first reacted in a Diels-Alder reaction with a cyclic 1,4-diene of formula (B) wherein R, R, Rand Rmay be, inter alia, hydrogen and Y may be, inter alia, —CH((i)-CH)—, to form a 5-nitro-benzonorbornadiene compound of formula (C). Subsequent catalytic reduction under standard conditions (for example, Ra/Ni or ...

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26-09-2013 дата публикации

PROCESS FOR PREPARING 3-AMINOMETHYL-3,5,5-TRIMETHYLCYCLOHEXYLAMINE

Номер: US20130253226A1
Принадлежит: EVONIK DEGUSSA GmbH

The invention relates to an improved process for preparing 3-aminomethyl-3,5,5-trimethylcyclohexylamine, referred to hereinafter as isophoronediamine or, in abbreviated form, IPDA, by: I. preparation of isophorone by catalyzed aldol condensations with acetone as reactant; II. reaction of isophorone with HCN to form isophoronenitrile (IPN, 3-cyano-3,5,5-trimethylcyclohexanone); III. catalytic hydrogenation and/or catalytic reductive amination (also referred to as aminative hydrogenation) of 3-cyano-3,5,5-trimethylcyclohexanone, hereinafter called isophoronenitrile or, in abbreviated form, IPN, to give the isophoronediamine. 1. A process for preparing isophoronediamine IPDA , the process comprising:(i) reacting acetone via a catalyzed aldol condensation in a reactor, thereby obtaining a reaction product comprising isophorone,(ii) working-up the reaction product, thereby obtaining a stream of value(iii) hydrolyzing the stream of value in a hydrolysis apparatus,(iv) separating the stream of value into an organic fraction and an aqueous fraction,(v) recovering isophorone from the organic fraction,(vi) distilling the aqueous fraction in a distillative workup apparatus comprising a top and a bottom,(vii) passing vapors from the top of the distillative workup apparatus onward into the hydrolysis apparatus,(viii) reacting isophorone with HCN via a base-catalyzed reaction, thereby obtaining isophoronenitrile IPN, and(ix) reacting IPN via a catalytic hydrogenation, a catalytic reductive amination, or both in the presence of ammonia, hydrogen, at least one catalyst, and optionally a solvent or a solvent mixture, thereby obtaining IPDA,wherein a cyanide ion concentration in a reaction mixture sent to the catalytic hydrogenation is of from 200 ppmw to 5000 ppmw, based on the IPN used.2. The process of claim 1 , wherein water from the bottom of the distillative workup apparatus is subjected to a flash evaporation claim 1 , thereby obtaining a purified water which is recycled into ...

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03-10-2013 дата публикации

Process for the Preparation of Iosimenol

Номер: US20130261338A1
Принадлежит: Mallinckrodt LLC

A process for the preparation of iosimenol comprising reacting 5,5′-[(1,3-dioxo-1,3-propanediyl)diimino]bis[N-(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide] (C-VI) with a 3-halo-1,2-propanediol in an aqueous solvent. A process for the preparation of C-VI comprising reacting 3,3′4(1,3-dioxo-1,3-propanediyl)diimino]bis[5-(aminocarbonyl)-2,4,6-triiodobenzoyl chloride] (C-V) with 3-amino-1,2-propanediol in the presence of an inorganic base and a suitable non-aqueous polar solvent. A process for the preparation of C-V comprising reacting 3-amino-5-(aminocarbonyl)-2,4,6-triiodobenzoyl chloride (C-IV) with malonyl dichloride in a solvent comprising a suitable ester solvent, a suitable nitrile solvent or mixtures thereof. 121-. (canceled)23. The process of wherein the solvent further comprises a suitable ethereal solvent.24. The process of wherein the solvent optionally further comprises a suitable ethereal solvent claim 22 , and the solvent is selected from acetonitrile claim 22 , ethyl acetate claim 22 , a mixture of acetonitrile and tetrahydrofuran claim 22 , a mixture of ethyl acetate and tetrahydrofuran claim 22 , a mixture of acetonitrile and 1 claim 22 ,2-dimethoxyethane claim 22 , a mixture of ethyl acetate and 1 claim 22 ,2-dimethoxyethane claim 22 , or a mixture of acetonitrile and ethyl acetate.25. The process of wherein the solvent is selected from acetonitrile claim 24 , ethyl acetate claim 24 , a mixture of acetonitrile and tetrahydrofuran claim 24 , a mixture of ethyl acetate and tetrahydrofuran claim 24 , or a mixture of acetonitrile and ethyl acetate.26. The process of wherein the solvent comprises acetonitrile or a mixture of acetonitrile and tetrahydrofuran.27. The process of wherein the solvent is a mixture of acetonitrile and tetrahydrofuran wherein the weight ratio of acetonitrile:tetrahydrofuran is about 1:9 to about 49:1.28. The process of wherein the weight ratio of acetonitrile:tetrahydrofuran is about 1:1 to about 49:1.29. The ...

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03-10-2013 дата публикации

PROCESS FOR PREPARING 3-AMINOMETHYL-3,5,5-TRIMETHYLCYCLOHEXYLAMINE

Номер: US20130261341A1
Принадлежит: EVONIK DEGUSSA GmbH

The invention relates to an improved process for preparing 3-aminomethyl-3,5,5-trimethylcyclohexylamine, referred to hereinafter as isophoronediamine or IPDA for short, by means of catalytic hydrogenation and/or catalytic reductive amination (also referred to as aminating hydrogenation) of -cyano--trimethylcyclohexanone, also called isophoronenitrile or IPN for short hereinafter. 1. A process for preparing isophoronediamine , the process comprising:hydrogenating, reductively aminating, or both hydrogenating and reductively aminating isophoronenitrile, in a presence of ammonia, hydrogen, a catalyst and optionally a solvent or a solvent mixture,wherein a cyanide ion concentration in a reaction mixture sent to the hydrogenating is of from 200 ppmw to 5000 ppmw, based on an amount of the isophoronenitrile added.2. The process of claim 1 ,wherein the cyanide ion concentration is of from 200 ppmw to 3000 ppmw.3. The process of claim 1 ,wherein the cyanide ion concentration is adjusted by controlled metered addition of HCN or a cyanide salt, or with an isophoronenitrile quality having the cyanide ion concentration of from 200 ppmw to 5000 ppmw.4. The process of claim 1 ,wherein an adjustment of the cyanide ion concentration is achieved by controlled redissociation of the isophoronenitrile in an imination stage.5. The process of claim 4 ,wherein the adjustment of the cyanide ion concentration by increasing a temperature in the imination stage by 5-50 K, above a temperature, depending on a presence of an imination catalyst, is needed to achieve a conversion of isophoronenitrile to isophoronenitrileimine of at least 80% in the imination stage.6. The process of claim 1 ,wherein the process is performed in one stage or a plurality of stages.7. The process of claim 1 ,wherein the isophoronediamine is prepared in a two-stage process.8. The process of claim 7 ,wherein the isophoronenitrile is partially converted to isophoronenitrileimine in a first stage by reacting with the ...

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10-10-2013 дата публикации

METHOD FOR PREPARING 2-AMINO-N-(2,2,2-TRIFLUOROETHYL) ACETAMIDE

Номер: US20130267729A1
Автор: Bruening Joerg
Принадлежит: E.I. Du Pont De Nemours and Company

Disclosed are methods for preparing compounds of Formula 1 and 1A. The first method utilizes a benzyl carbamate amine protecting group and an intermediate of Formula 4. The second method utilizes a tert-butyl carbamate amine protecting group and an intermediate of Formula 7. The third method utilizes a dibenzyl amine protecting group. Also disclosed is a compound, phenylmethyl N-[2-oxo-2-[(2,2,2-trifluoroethyl)amino]ethyl]carbamate (a compound of Formula 4). Further disclosed is a method for preparing a compound of Formula 14 from a compound of Formula 15 and a compound of Formula 1 or 1A. 2. The method of step (A) wherein the compounds of Formulae 2 and 3 and the coupling reagent are contacted in the presence of a base and a water immiscible solvent.3. The method of wherein the base is derived from the coupling reagent and the coupling reagent is N claim 2 ,N′-carbonyldiimidazole.4. The method of step (B) wherein the compound of Formulae 4 and hydrogen are contacted in the presence of a hydrogenolysis catalyst and a water immiscible solvent.5. The method of wherein the hydrogenolysis catalyst is palladium on carbon.6. The method of step (C) wherein the compound of Formula 1 is contacted with an acid of Formula 5 in the presence of a water immiscible solvent.7. The method of wherein the acid of Formula 5 comprises hydrogen chloride.8. (canceled)9. A compound which is phenylmethyl N-[2-oxo-2-[(2 claim 6 ,2 claim 6 ,2-trifluoroethyl)amino]-ethyl]carbamate.11. The method of step (A1) wherein the compounds of Formulae 8 and 3 and the coupling reagent are contacted in the presence of a base and a water immiscible solvent.12. The method of wherein the base is derived from the coupling reagent and the coupling reagent is N claim 11 ,N′-carbonyldiimidazole.13. The method of step (B1) wherein the compounds of Formulae 7 and 5 are contacted in the presence of a water immiscible solvent.14. The method of wherein the acid of Formula 5 comprises hydrogen chloride.15. (canceled) ...

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17-10-2013 дата публикации

PROCESSES FOR SEPARATING ONE OR MORE AMINE BYPRODUCTS FROM ONE OR MORE DESIRED AMINES

Номер: US20130274522A1
Принадлежит: Dow Global Technologies LLC

The present invention relates to separating one or more amine byproducts from one or more desired amines. More particularly, the invention involves forming a byproduct component with one or more amine byproducts and a first adjuvant component. The byproduct component has an enhanced separation characteristic relative to separating the amine byproducts from the desired amines in the absence of an adjuvant. Preferably, the byproduct component is separated in the presence of a second adjuvant component that preferably has a boiling point less than the boiling point of the first adjuvant component.

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24-10-2013 дата публикации

P-terphenyl compound mixture and electrophotographic photoreceptors made by using the same

Номер: US20130280652A1
Принадлежит: Hodogaya Chemical Co Ltd

An object of the invention is to provide a method of making a p-terphenyl compound mixture which includes two symmetric p-terphenyl compounds respectively represented by formula (1) and formula (2) and an asymmetric p-terphenyl compound represented by formula (3)

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24-10-2013 дата публикации

FINGOLIMOD POLYMORPHS AND THEIR PROCESSES

Номер: US20130281739A1
Принадлежит:

The present invention provides crystalline polymorphic forms of Fingolimod HCl (I) and processes for preparation thereof. 1. Fingolimod hydrochloride crystalline Form-α characterized by X-ray powder diffraction pattern comprising at least 5 characteristic 2θ° peaks selected from the XRPD peak set of 10.51 , 15.20 , 19.27 , 21.77 , 23.12 , 24.91 , 26.14 , 26.46 , 29.03 , 33.47 and 35.46±0.1 2θ°.21. Fingolimod hydrochloride crystalline Form-α according to claim- , which is further characterized by DSC isotherm comprising at least three endothermic peaks ranging between—a. Peak-1—Between 40 to 43° C.b. Peak-2—Between 65 to 68° C.c. Peak-3—Between 105 to 110° C.d. Peak-4—Between 270 to 280° C.3. Fingolimod hydrochloride crystalline Form-α characterized by X-ray powder diffraction pattern comprising at least 5 characteristic 2θ° peaks selected from the XRPD peak set of 10.51 , 15.20 , 19.27 , 21.77 , 23.12 , 24.91 , 26.14 , 26.46 , 29.03 , 33.47 and 35.46±0.1 2θ° and DSC isotherm comprising the endothermic peaks ranging between 40 to 43° C. (Peak-1) , 65 to 68° C. (Peak-2) , 105 to 110° C. (Peak-3) and/or 270 to 280° C. (Peak-4).43. Fingolimod hydrochloride crystalline Form-α according to claim- , characterized by X-ray powder diffraction pattern substantially according to and DSC isothermal pattern substantially according to .5. A process for preparing Fingolimod hydrochloride crystalline Form-α comprising the steps of—a. Combining the Fingolimod hydrochloride with an organic acidb. Optionally heating up to about 40-50° C.c. cooling the solution up to about 0-5° C.d. isolating the crystalline Form-α.6. A process for preparing Fingolimod hydrochloride crystalline Form-α according to claim 5 , wherein organic acid may be selected from C1 to C4 carboxylic acids.7. Fingolimod hydrochloride crystalline Form-β characterized by X-ray powder diffraction pattern comprising at least 4 characteristic 2θ° peaks selected from the XRPD peak set of 3.54 claim 5 , 7.07 claim 5 , 10.66 ...

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31-10-2013 дата публикации

Process for Isomerization of CIS-2-Pentenenitrile to 3-Pentenenitriles

Номер: US20130289299A1
Принадлежит: BASF SE

The present invention relates to an improved process for batchwise or continuous isomerization of cis-2-pentenenitrile to 3-pentenenitriles in the presence of 1,4-diazabicyclo[2.2.2]octane as catalyst. 16-. (canceled)7. A process for batchwise or continuous isomerization of cis-2-pentenenitrile to 3-pentenenitriles , which comprises isomerizing cis-2-pentenenitrile with 1 ,4-diazabicyclo[2.2.2]octane.8. The process according to claim 7 , wherein cis-2-pentenenitrile is isomerized at temperatures of 80 to 200° C. and a pressure of 0.01 to 50 bar.9. The process according to claim 7 , wherein the isomerization of cis-2-pentenenitrile to 3-pentenenitriles is performed in a reaction column.10. The process according to claim 7 , whereina) 3-pentenenitriles or a mixture comprising 3-pentenenitriles is/are hydrocyanated to adiponitrile in the presence of nickel(0)-phosphorus ligand complexes as catalysts,b) adiponitrile, 2-methylglutaronitrile and nickel(0)-phosphorus ligand complex are removed from the hydrocyanation output,c) the cis-2-pentenenitrile in the thus obtained organic phase comprising unsaturated C5 mononitriles is isomerized to 3-pentenenitriles with the aid of 1,4-diazabicyclo[2.2.2]octane as a catalyst, which has a higher boiling point at standard pressure than cis-2-pentenenitrile,whereind) the organic phase which comprises essentially unsaturated C5 mononitriles and is obtained in c) is supplied to a distillation column K1, cis-2-pentenenitrile and cis- and trans-2-methyl-2-butenenitrile are removed from the distillation column K1 via the top, and 3-pentenenitrile and trans-2-pentenenitrile are removed from the distillation column K1 via the bottom, and the latter are recycled into the reaction step for hydrocyanation of 3-pentenenitriles,e) the top product from the distillation column K1 is fed to a distillation column K2, and trans-2-methyl-2-butenenitrile is removed and discharged as a bottom product of column K2,f) a top product from column K2 and 1,4- ...

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