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    PRODUCTION OF OPTICALLY ACTIVE ALPHA-AMINO-EPSILON-CAPROLACTAM
    83.
    发明专利
    PRODUCTION OF OPTICALLY ACTIVE ALPHA-AMINO-EPSILON-CAPROLACTAM 失效

    公开(公告)号：JPS62114970A

    公开(公告)日：1987-05-26

    申请号：JP25491585

    申请日：1985-11-15

    Applicant: TORAY INDUSTRIES

    Inventor： MIYATA AKIRA ,  IMAMURA SHINZO

    IPC: C07B57/00 ,  C07B31/00 ,  C07C67/00 ,  C07D223/12

    Abstract: PURPOSE:To obtain the titled compound in high yield and optical purity with simple procedure, by carrying out the optical resolution of DL-alpha-amino-epsilon- caprolactam using an optically active alanine derivative as an optical resolution agent. CONSTITUTION:1mol of DL-alpha-amino-epsilon-caprolactam (abbreviated as DL-ACL) is made to contact with 0.1-2.0mol of at least one kind of alanine derivative selected from N-formylphenylalanine and N-acetyl-phenylalanine as an optical resolution agent at 0-80 deg.C preferably in water. A hardly soluble diastereomer salt is crystallized from the resultant solution e.g. by cooling the solution. The salt is separated by a solid-liquid separation process such as filtration, centrifugal separation, etc., and is subjected to optical resolution e.g. by contacting with a cation exchange resin in an aqueous solvent. The resolution agent is separated and the cation exchange resin is eluted with NH3, etc., to obtain D-ACL or L-ACL useful as an intermediate for L-lysine or raw material of pharmaceuticals such as hypotensor.

    PRODUCTION OF ORGANIC DICARBOXYLIC ESTER
    86.
    发明专利
    PRODUCTION OF ORGANIC DICARBOXYLIC ESTER 失效

    公开(公告)号：JPH11302222A

    公开(公告)日：1999-11-02

    申请号：JP13120798

    申请日：1998-04-24

    Applicant: TORAY INDUSTRIES ,  SODA AROMATIC

    Inventor： MURAOKA HIDEO ,  IMAMURA SHINZO ,  TAKAOKA HIDEAKI ,  ITO NOBUHIKO ,  HASEBE AKIO

    IPC: B01J31/08 ,  C07B61/00 ,  C07C67/08 ,  C07C69/34

    Abstract: PROBLEM TO BE SOLVED: To provide a process for simply and efficiently producing organic dicarboxylic esters of industrially excellent quality by using a reduced amount of alcohol. SOLUTION: In the esterification reaction between an organic dicarboxylic acid of the general formula I: HOOC-R -COOH and a monohydric alcohol of the general formula II: HO-R -OH in the presence of a solid acid catalyst through the continuous flow reactor system, the organic dicarboxylate ester as the esterification reaction product is kept together with these reactants of the organic dicarboxylic acid and the monohydric alcohol to homogenize their mixture followed by esterification thereby producing the objective organic dicarboxylic ester of the general formula III:R OOC-R -COOR (R is a 6-14 C straight of branched hydrocarbon; R is a 1-4 C straight or branched hydrocarbon).

    SEPARATION AND PURIFICATION OF 2-(OMEGA-ALKOXYCARBONYLALKANOYL)-4-BUTANOLIDE ALKALI METAL SALT AND ITS DERIVATIVE AND DICARBOXYLIC ACID ESTER
    87.
    发明专利
    SEPARATION AND PURIFICATION OF 2-(OMEGA-ALKOXYCARBONYLALKANOYL)-4-BUTANOLIDE ALKALI METAL SALT AND ITS DERIVATIVE AND DICARBOXYLIC ACID ESTER 失效

    公开(公告)号：JPH1192472A

    公开(公告)日：1999-04-06

    申请号：JP21068498

    申请日：1998-07-27

    Applicant: SODA AROMATIC ,  TORAY INDUSTRIES

    Inventor： TAKAOKA HIDEAKI ,  ITO NOBUHIKO ,  HASEBE AKIO ,  IMAMURA SHINZO

    IPC: C07D307/33 ,  C07C67/343 ,  C07C67/58 ,  C07C69/716

    Abstract: PROBLEM TO BE SOLVED: To industrially and advantageously separate and purify a 2-(ω- alkoxycarbonylalkanoyl)-4-butanolide alkali metal salt and its derivative and an reacted ester simply and in a high yield from a condensation reaction solution obtained by reacting a dicarboxylic acid ester with γ-butyrolactone. SOLUTION: In this method for separating a 2-(ω-alkoxycarbonylalkanoyl)-4- butanolide alkali metal salt of the formula ((n) is 7-13; R is a 1-6C alkyl group; M is an alkali metal) and its derivative and an unreacted dicarboxylic acid ester from a condensation reaction solution obtained by reacting θ-butyrolactone with a dicarboxylic acid ester of the general formula (1) ROOC(CH2 )n COOR ((n) is 7-13; R is a 1-6C alkyl group), a solid-liquid separation is carried out by using an inert solvent or an extraction is performed by using water or an alkali aqueous solution to separate and purify both the 2-(ω- alkoxycarbonylalkanoyl)-4-butanolide alkali metal salt and its derivative and the unreacted dicarboxylic acid ester.

    PRODUCTION AND STORAGE OF HIGH GRADE PYRUVIC ACID ESTER
    88.
    发明专利
    PRODUCTION AND STORAGE OF HIGH GRADE PYRUVIC ACID ESTER 失效

    公开(公告)号：JPH10330318A

    公开(公告)日：1998-12-15

    申请号：JP14429297

    申请日：1997-06-02

    Applicant: TORAY INDUSTRIES

    Inventor： ONO TAKAE ,  IMAMURA SHINZO

    IPC: C07C67/54 ,  C07C69/716

    Abstract: PROBLEM TO BE SOLVED: To obtain the subject compound having high quality. SOLUTION: A high grade pyruvic acid ester obtained by distillation using a distillation tower having a capacity of an effective plate number of 1 or more, is transferred to a container for storage or carry as soon as possible, closed tightly, followed by keeping its temperature at a value or lower which is calculated from the following equation: log D=(2.75/(t+273)×10 -6.73, wherein D (d) is a storage time for carry, etc.; t ( deg.C) is the temperature controlled.

    PRODUCTION OF P-HYDROXYBENZOIC ACID
    89.
    发明专利
    PRODUCTION OF P-HYDROXYBENZOIC ACID 失效

    公开(公告)号：JPH1087558A

    公开(公告)日：1998-04-07

    申请号：JP23949296

    申请日：1996-09-10

    Applicant: TORAY INDUSTRIES

    Inventor： ENDO ITARU ,  IMAMURA SHINZO

    IPC: C07C51/15 ,  C07C65/03

    Abstract: PROBLEM TO BE SOLVED: To obtain p-hydroxybenzoic acid useful as a raw material of a medicine or an agrochemical agent, by reacting an alkali metal salt of phenol with carbon dioxide in an aprotic polar solvent in the presence of an alkali metal salt of a compound having a weak acidity. SOLUTION: This method for producing p-hydroxybenzoic acid is to react an alkali metal salt of phenol with carbon dioxide in an aprotic polar solvent in the presence of an alkali metal salt of a weakly acidic compound of formula I (M is Na or K; R to R are each H or a 1-12C alkyl) or formula II (R , R are each H or a 1-12C alkyl), etc. Further, as the coexisting alkali metal salt, it is preferable to use the salt not reacting with carbon dioxide by >=1.5% in reacting at 70 deg.C at 1.5MPa carbon dioxide pressure for 4hr.

    PRODUCTION OF AZO COMPOUND
    90.
    发明专利
    PRODUCTION OF AZO COMPOUND 失效

    公开(公告)号：JPH09157240A

    公开(公告)日：1997-06-17

    申请号：JP33812095

    申请日：1995-12-01

    Applicant: TORAY INDUSTRIES

    Inventor： NAKANO KEIKO ,  IMAMURA SHINZO

    IPC: C07C245/08 ,  C09B41/00

    Abstract: PROBLEM TO BE SOLVED: To obtain an azo compound by a process advantageous from the operational and economical points of view by dispersing solid particles of a phenolic compound in water in the presence of a surfactant and subjecting the phenolic compound to a coupling reaction. SOLUTION: (A) A phenolic compound exhibiting solid particle form is made to react with (B) diazonium salt of an aromatic aniline compound in the presence of (C) a surfactant in water to obtain (D) the objective azo compound. Preferably, the component A is a phenolic compound of formula I (R1 is H, a 1-12C alkyl, a 5-6C cycloalkyl, phenyl, etc.; R2 is H, a halogen, OH or a 1-4C alkoxy; R3 is a halogen, a 1-12C alkyl, a 5-6C cycloalkyl, a 1-4C alkoxy, phenyl, etc.), the component B is an aromatic aniline compound of formula II (R4 is H, a halogen, a 1-12C alkyl, carboxy, etc.) and the component D is an azo compound of formula III.

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