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公开(公告)号：HU9303396D0
公开(公告)日：1994-03-28
申请号：HU9303396
申请日：1993-11-30
Applicant: TORAY INDUSTRIES
Inventor： SATO HARUYO , NAKAI SAKIE , FUJINO TOSHIHIRO
IPC: C07D307/56 , C07C67/52 , C07C69/70 , C07C69/76 , C07C69/78
Abstract: Crystals of an aromatic 0,0'-diacyltartaric acid of the formula (VIII): wherein R and R are the same as or different from one another and each is a hydrogen atom, halogen atom or C1 - C4 alkyl group are sufficiently uniform in size that 95% to 98% of them pass through a 20-mesh sieve. Such crystals may be prepared by hydrolyzing an aromatic carboxylic anhydride of the formula (IV): wherein R and R are as defined above, to form the corresponding acid (VIII) in the form of an oil and crystallizing the acid in the presence of an organic solvent which is immiscible with water to form crystals of the hydrate of the acid (VIII). For the crystallization process, each of the organic solvent immiscible with water and seed crystals of the acid (VIII) are added to the oil of the acid (VIII) present in the reaction mixture.
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公开(公告)号：DE69326050T2
公开(公告)日：2000-02-03
申请号：DE69326050
申请日：1993-11-30
Applicant: TORAY INDUSTRIES
Inventor： SATO HARUYO , NAKAI SAKIE , FUJINO TOSHIHIRO
Abstract: Crystals of an aromatic 0,0'-diacyltartaric acid of the formula (VIII): wherein R and R are the same as or different from one another and each is a hydrogen atom, halogen atom or C1 - C4 alkyl group are sufficiently uniform in size that 95% to 98% of them pass through a 20-mesh sieve. Such crystals may be prepared by hydrolyzing an aromatic carboxylic anhydride of the formula (IV): wherein R and R are as defined above, to form the corresponding acid (VIII) in the form of an oil and crystallizing the acid in the presence of an organic solvent which is immiscible with water to form crystals of the hydrate of the acid (VIII). For the crystallization process, each of the organic solvent immiscible with water and seed crystals of the acid (VIII) are added to the oil of the acid (VIII) present in the reaction mixture.
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公开(公告)号：HUT69765A
公开(公告)日：1995-09-28
申请号：HU9303396
申请日：1993-11-30
Applicant: TORAY INDUSTRIES
Inventor： SATO HARUYO , NAKAI SAKIE , FUJINO TOSHIHIRO
IPC: C07D307/56 , C07C67/52 , C07C69/70 , C07C69/76 , C07C69/78 , C07D307/60
Abstract: Crystals of an aromatic 0,0'-diacyltartaric acid of the formula (VIII): wherein R and R are the same as or different from one another and each is a hydrogen atom, halogen atom or C1 - C4 alkyl group are sufficiently uniform in size that 95% to 98% of them pass through a 20-mesh sieve. Such crystals may be prepared by hydrolyzing an aromatic carboxylic anhydride of the formula (IV): wherein R and R are as defined above, to form the corresponding acid (VIII) in the form of an oil and crystallizing the acid in the presence of an organic solvent which is immiscible with water to form crystals of the hydrate of the acid (VIII). For the crystallization process, each of the organic solvent immiscible with water and seed crystals of the acid (VIII) are added to the oil of the acid (VIII) present in the reaction mixture.
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公开(公告)号：IN187246B
公开(公告)日：2002-03-09
申请号：IN2997MA1997
申请日：1997-12-26
Applicant: TORAY INDUSTRIES
Inventor： SATO MARUYO , NAKAI SAKIE , FUNBASHI KEIKO , IWATA SHIHO
IPC: C07C49/00
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公开(公告)号：DE69326050D1
公开(公告)日：1999-09-23
申请号：DE69326050
申请日：1993-11-30
Applicant: TORAY INDUSTRIES
Inventor： SATO HARUYO , NAKAI SAKIE , FUJINO TOSHIHIRO
Abstract: Crystals of an aromatic 0,0'-diacyltartaric acid of the formula (VIII): wherein R and R are the same as or different from one another and each is a hydrogen atom, halogen atom or C1 - C4 alkyl group are sufficiently uniform in size that 95% to 98% of them pass through a 20-mesh sieve. Such crystals may be prepared by hydrolyzing an aromatic carboxylic anhydride of the formula (IV): wherein R and R are as defined above, to form the corresponding acid (VIII) in the form of an oil and crystallizing the acid in the presence of an organic solvent which is immiscible with water to form crystals of the hydrate of the acid (VIII). For the crystallization process, each of the organic solvent immiscible with water and seed crystals of the acid (VIII) are added to the oil of the acid (VIII) present in the reaction mixture.
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Patent Agency Ranking
公开(公告)号：JPH09151159A
公开(公告)日：1997-06-10
申请号：JP31403995
申请日：1995-12-01
Applicant: TORAY INDUSTRIES
Inventor： IWATA SHIHO , NAKAI SAKIE , SATOU HARUYO
IPC: C07B55/00 , C07C51/347 , C07C57/58 , C07C59/50
Abstract: PROBLEM TO BE SOLVED: To obtain a racemic carboxylic acid useful as an intermediate raw material for medicines and agrochemicals in high yield by reducing the amount of a base used and racemizing an optically active carboxylic acid under mild conditions. SOLUTION: The racemizing reaction of an optically active carboxylic acid represented by the formula (R and R are each hydroxyl, a 1-10C alkyl, a 6-10C aryl, a 7-11C aralkyl or a 5-6C cycloalkyl; X is H or an alkali metal) or an alkali metallic salt thereof is carried out in the coexistence of a base (e.g. potassium hydroxide) and dimethyl sulfoxide at 60-130 deg.C for 0.1-40hr. The base is used in an amount of 1.01-10 equiv. based on the optically active carboxylic acid and 0.01-9 equiv. based on the alkali metallic salt of the optically active carboxylic acid. The dimethyl sulfoxide is used in an amount of 0.1-10 times based on the optically active carboxylic acid (alkali metallic salt). An organic solvent (e.g. cyclohexane) and water may coexist in racemization.
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公开(公告)号：JPH04108766A
公开(公告)日：1992-04-09
申请号：JP22735790
申请日：1990-08-28
Applicant: TORAY INDUSTRIES
Inventor： NAKAI SAKIE , SATOU HARUYO
IPC: C07C209/88 , C07B57/00 , C07C211/27
Abstract: PURPOSE:To optically resolve (RS)-1-methyl-3-phenylpropylamine by extremely simple method and in good yield and in high optical purity, using an optically active N-formylphenylglycin as a resolving agent. CONSTITUTION:1mol (RS)-1-methyl-3-phenylpropylamine is brought into contact with 0.1-2.0mol, preferably 0.3-1.0mol N-formyl-D-phenylglycin or N-formyl-L- phenylglycin in a solvent, preferably water or ethanol to produce two kinds of diastereomer salts. The solution is cooled and/or concentrated to crystallize a hardly soluble diastereomer salt and the diastereomer is separated and collected according to an ordinary solid-liquid separation method. The separated diastereomer salt is treated with an acid or alkali. Thereby, optically active objective compound is obtained and simultaneously optically active N- formylphenylglycin is recovered and re-used.
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公开(公告)号：JPH1087536A
公开(公告)日：1998-04-07
申请号：JP23949096
申请日：1996-09-10
Applicant: TORAY INDUSTRIES
Inventor： SATOU HARUYO , NAKAI SAKIE
Abstract: PROBLEM TO BE SOLVED: To make it possible to obtain inexpensively, simply and efficiently an alicyclic alcohol of high optical purity, which is useful as raw material for medicines and agrochemicals, by subjecting an tartaric ester to diastereomer splitting followed by hydrolysis. SOLUTION: A compound of the formula each of R and R are a 1-4C alkyl carbonyl, phenyl, a (1-4C alkyl, halogen-substituted) aryl-carbonyl; R is [1-4C alkyl, alkoxy, (1-4C alkyl, halogen-substituted) phenyl, aralkyl- substituted] alicyclic alkyl; the tartaric skeleton is (R, R) configuration or (S, S) configuration} is subjected to the diastereomer splitting through crystallization, column separation, simulated moving bed separation to obtain an optically active tartaric ester followed by hydrolysis.
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公开(公告)号：JPH0859517A
公开(公告)日：1996-03-05
申请号：JP13462295
申请日：1995-06-01
Applicant: TORAY INDUSTRIES
Inventor： NAKAI SAKIE , SATOU HARUYO , FUJINO TOSHIHIRO
IPC: C07D307/24 , C07B57/00
Abstract: PURPOSE: To enable a practically advantageous production of optically active tetrahydrofurancarboxylic acid which is useful as an intermediate for medicines by using a chemically modified optically active amino acid inexpensively available as an agent for optical resolution. CONSTITUTION: An agent for optical resolution of tetrahydrofurancarboxylic acid, that is, an optically active amino acid amide. The agents of formula I or formula II (R1 is an alkyl, an aryl, an aralkyl; R2 , R3 are each an alkyl, an aryl, an aralkyl; R4 is a cyclic alkylamine residue) are preferred. The agent is used to effect the optical resolution to give optically active tetrahydrofuran- carboxylic acid. As an optically active amino acid amide derivative, is cited particularly optically active alanine benzyl-amide, optically active alanine anilide, optically active phenyl-alanine amide or the like. As the tetrahydrofurancarboxylic acid. tetrahydrofuran-2-carboxylic acid is particularly desirable. This agent for optical resolution can be used repeatedly.
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公开(公告)号：JPH07188123A
公开(公告)日：1995-07-25
申请号：JP33118493
申请日：1993-12-27
Applicant: TORAY INDUSTRIES
Inventor： SATOU HARUYO , NAKAI SAKIE
IPC: C07B57/00 , C07C209/88 , C07C211/36
Abstract: PURPOSE:To produce an optically active trans DACH suitable for industrial use from a mixture containing cis DACH and trans DACH and available as an inexpensive raw material. CONSTITUTION:This process for the production of an optically active trans-1,2- diaminocyclohexane comprises (A) an optical resolution step to separate an optically active tartaric acid salt of an optically active trans-1,2- diaminocyclohexane in the form of crystal from a mixture containing trans-1,2 diaminocyc1ohexane and cis-1,2-diaminocyclohexane in an aqueous solvent by adding D or L-tartaric acid as a resolution agent to the mixture without separating the trans-1,2-diaminocyclohexane from the mixture, (B) a salt-dissociation step to contact the resolved crystal of (A) with an inorganic alkali in an alcohol solution, transfer the isolated (R,R)-1,2-diaminocyclohexane or (S,S)-1,2- diaminocyclohexane into the alcohol and recover the precipitated optically active alkali tartrate by solid-liquid separation and (C) a step to recycle the recovered salt of (B) to the resolution step (A).
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