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    PURIFICATION OF OMEGA-FORMYLCARBOXYLIC ACID ESTER
    31.
    发明专利
    PURIFICATION OF OMEGA-FORMYLCARBOXYLIC ACID ESTER 失效

    公开(公告)号：JPH0920722A

    公开(公告)日：1997-01-21

    申请号：JP17173395

    申请日：1995-07-07

    Applicant: UBE INDUSTRIES

    Inventor： KAKEYA NOBORU ,  TAKAI TSUTOMU

    IPC: B01J27/08 ,  B01J31/22 ,  C07B61/00 ,  C07C67/42 ,  C07C67/475 ,  C07C69/67

    Abstract: PROBLEM TO BE SOLVED: To readily obtain an ω-formylcarboxylic acid ester useful in various fields as a main product in high yield by reacting a cycloalkanone with a nitrous acid ester in the presence of a Lewis acid. SOLUTION: (A) A cycloalkanone (e.g. cyclopentanone or cyclohexanone) is reacted with (B) a nitrous acid ester (e.g. methyl nitrite, ethyl nitrite, n-butyl nitrite or i-butyl nitrite) in the presence of a Lewis acid (preferably a boron trifluoride methanol complex, a boron trifluoride ether complex, etc.), preferably at -10 to +30 deg.C to afford (C) an ω-formylcarboxylic acid ester of the formula [R is a 1-6C alkyl or a 5-8C cycloalkyl; (n) is an integer of 4-11]. Furthermore, the component (B) is used in an amount of 1-8 equiv., preferably 2-5 equiv. based on the component (A). The Lewis acid is used in an amount of 0.01-0.5 equiv., preferably 0.05-0.1 equiv. based on the component (A).

    PRODUCTION OF 2-HYDROXYCYCLOHEXANONE OXIME
    32.
    发明专利
    PRODUCTION OF 2-HYDROXYCYCLOHEXANONE OXIME 失效

    公开(公告)号：JPH093026A

    公开(公告)日：1997-01-07

    申请号：JP15302695

    申请日：1995-06-20

    Applicant: UBE INDUSTRIES

    Inventor： KAKEYA NOBORU ,  ABE KOJI

    IPC: C07C249/06 ,  C07C251/44

    Abstract: PURPOSE: To easily obtain the subject compound useful as a raw material for 5-cyanopentanal, which is the precursor of ε-caprolactam, in a high yield by reacting 1-formyloxy or hydroxy-2-nitrosocyclohexane with an organic base and an alcohol or water. CONSTITUTION: This method for producing 2-hydroxycyclohexane oxime comprises reacting (A) 1-formyloxy-2-nitrosocyclohexane or 1-hydroxy-2- nitrosocyclohexane with (B) an organic base such as a 3-13C aliphatic tertiary amine compound or a pyridine compound and (C) an alcohol or water e.g. in amounts of 1-10 equivalents and 1-300wt. times, respectively, based on the component A. The reaction is preferably performed in a reaction solvent such as acetonitrile at 70-100 deg.C under the atmospheric pressure or an elevated pressure.

    PRODUCTION OF 1,6-DIOXYIMINOHEXANE
    33.
    发明专利
    PRODUCTION OF 1,6-DIOXYIMINOHEXANE 失效

    公开(公告)号：JPH093024A

    公开(公告)日：1997-01-07

    申请号：JP15302495

    申请日：1995-06-20

    Applicant: UBE INDUSTRIES

    Inventor： KAKEYA NOBORU ,  ABE KOJI

    IPC: C07C249/06 ,  C07C249/04 ,  C07C251/38 ,  C07C251/44

    Abstract: PURPOSE: To highly easily obtain the subject compound useful as a raw material for producing hexamethylenediamine, which is a raw material for nylon 66, in a high yield by reacting 1-formyloxy or hydroxy-2-nitrosocyclohexane with an inorganic base. CONSTITUTION: This method for producing 1,6-dioxyiminohexane comprises reacting (A) 1-formyloxy-2-nitrosocyclohexane or 1-hydroxy-2-nitrosocyclohexane with (B) an inorganic base such as the hydroxide, (bi)carbonate, etc., of an alkali(ne earth) metal e.g. in an amount of 1-10 equivalents based on the component A in terms of the monomer. The reaction is preferably performed in a reaction solvent such as a 1-4C aliphatic alcohol or water at 70-100 deg.C under the atmospheric pressure or an elevated pressure.

    PRODUCTION OF CYCLODODECYLAMINE
    34.
    发明专利
    PRODUCTION OF CYCLODODECYLAMINE 失效

    公开(公告)号：JPH06247906A

    公开(公告)日：1994-09-06

    申请号：JP3835293

    申请日：1993-02-26

    Applicant: UBE INDUSTRIES

    Inventor： HARADA KATSUMASA ,  KAKEYA NOBORU ,  FUJIMURA HITOSHI

    IPC: B01J23/44 ,  C07B61/00 ,  C07C209/40 ,  C07C211/35 ,  C07C249/06 ,  C07C251/44

    Abstract: PURPOSE:To produce cyclododecylamine in high selectivity and yield from 2-chlorocyclododecadienone oxime as a safe starting raw material easily synthesizable from cyclododecatriene. CONSTITUTION:The process for the production of cyclododecylamine is characterized by the use of 2-chlorocyclododecadienone oxime synthesized by the addition reaction of cyclododecatriene with nitrosyl chloride as a raw material and the hydrogenation of the oxime in the presence of a palladium catalyst at 60-160 deg.C.

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