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    PRODUCTION OF N-METHYLCAPROLACTAM
    21.
    发明专利
    PRODUCTION OF N-METHYLCAPROLACTAM 失效

    公开(公告)号：JPH01283273A

    公开(公告)日：1989-11-14

    申请号：JP11182788

    申请日：1988-05-09

    Applicant: TORAY INDUSTRIES

    Inventor： FUJINO TOSHIHIRO ,  MATSUKUMA YOSHIHISA

    IPC: C07D223/10 ,  C08K5/34 ,  C08K5/3412 ,  C09D7/12

    Abstract: PURPOSE:To obtain the subject compound useful as a polar aprotic solvent, etc., by reacting epsilon-caprolactam with methyl halide in the presence of an alkali metal hydroxide, adding water to the reaction mixture, separating into two layers and easily separating the objective compound from the organic layer. CONSTITUTION:epsilon-Caprolactam is made to react with a methyl halide in the presence of an alkali metal hydroxide at 30-80 deg.C. The amounts of the alkali metal hydroxide and the methyl halide are 0.5-3.0mol and 0.9-1.5mol per 1mol of the epsilon-caprolactam, respectively. The alkylation reaction mixture is separated into two layers in the presence of water and an alkali metal hydroxide and the objective compound is separated from the organic layer. The amount of water is preferably 1-5 times the total amount of the alkali metal halide and the alkali metal hydroxide in the alkylation reaction mixture. The amount of the alkali metal hydroxide to be added in the separation of the reaction mixture into two layers is 10-25wt.% based on water.

    PRODUCTION OF N-METHYLCAPROLACTAM
    22.
    发明专利
    PRODUCTION OF N-METHYLCAPROLACTAM 失效

    公开(公告)号：JPH01283272A

    公开(公告)日：1989-11-14

    申请号：JP11182688

    申请日：1988-05-09

    Applicant: TORAY INDUSTRIES

    Inventor： FUJINO TOSHIHIRO ,  MATSUKUMA YOSHIHISA

    IPC: C07D223/10 ,  C08K5/34 ,  C08K5/3412 ,  C09D7/12

    Abstract: PURPOSE:To produce the subject compound useful as a polar aprotic solvent, etc., in high purity and yield by reacting epsilon-caprolactam with a methyl halide, hydrolyzing the unreacted epsilon-caprolactam after the reaction and separating the objective compound from the reaction system. CONSTITUTION:epsilon-Caprolactam is made to react with a methyl halide in the presence of an alkali metal hydroxide at 10-100 deg.C, preferably 30-80 deg.C. The amounts of the alkali metal hydroxide and the methyl halide are 0.5-30mol and 0.9-1.5mol per 1mol of the epsilon-caprolactam, respectively. The objective compound is produced by hydrolyzing the unreacted epsilon-caprolactam. The hydrolysis reaction is performed by using the alkylation reaction liquid as it is. The water for hydrolysis is used preferably in an amount to enable the dissolution of the alkali metal halide and the alkali metal hydroxide contained in the raw material and the amount of the alkali metal hydroxide is preferably 1-50mol per 1 mol of the epsilon-caprolactam.

    DEVELOPING COMPOSITION FOR ELECTROSTATIC CHARGE IMAGE
    23.
    发明专利
    DEVELOPING COMPOSITION FOR ELECTROSTATIC CHARGE IMAGE 失效

    公开(公告)号：JPS63202761A

    公开(公告)日：1988-08-22

    申请号：JP3440587

    申请日：1987-02-19

    Applicant: FUJI XEROX CO LTD ,  TORAY INDUSTRIES

    Inventor： SUZUKI CHIAKI ,  MATSUMURA YASUO ,  AOKI TAKAYOSHI ,  NAKAOKA KENJI ,  MATSUKUMA YOSHIHISA

    IPC: G03G9/097

    Abstract: PURPOSE:To improve the dispersibility of the toner, and to reduce the scattering of electrification by incorporating a specific metal complex of cyclohexanone oxim in the titled composition, as the electrostatic charge controller to form the toner. CONSTITUTION:The titled composition contains the metal complex of cyclohexanone oxim shown by the formula as the charge controller. In the formula, R1 and R2 are each hydrogen atom, a substd. or an unsubstd. alkyl, aryl or aralkyl group. The metal complex compd. of the cyclohexanone oxim contains for example, 2-amino hexanone oxim, 2-methylamino hexanone oxim or 2-benzyl aminohexanone oxim, etc. as a ligand, and contains for example, iron, cobalt, nickel, chromium, manganese zinc, etc., as a metal. Thus, as the toner contains the cyclohexanone oxim derivative, the rising speed of the electrification increases, and the scattering of the frictional electrification is reduced.

    PRODUCTION OF ISOXAZOLE COMPOUND
    26.
    发明专利
    PRODUCTION OF ISOXAZOLE COMPOUND 失效

    公开(公告)号：JPS62111972A

    公开(公告)日：1987-05-22

    申请号：JP25085585

    申请日：1985-11-11

    Applicant: TORAY INDUSTRIES

    Inventor： ONO TAKAE ,  MATSUKUMA YOSHIHISA

    IPC: C07D261/14 ,  B01J23/00 ,  B01J23/04 ,  B01J27/232 ,  B01J27/26 ,  C07B61/00

    Abstract: PURPOSE:To obtain the titled compound useful as an intermediate for sulfa drugs in one step, by reacting an alpha-chloroxime salt or a mixture of the salt and its free oxime with a metal cyanide in the presence of sodium carbonate and/or sodium hydroxide. CONSTITUTION:The isoxazole compound of formula II (e.g. 5-amino-3,4- dimethylisoxazole) can be produced by reacting (A) an alpha-chloroxime salt of formula I (R and R are alkyl; X is acid residue) (e.g. 3-chloro-2-butanoxime hydrochloride) or a mixture of the salt and its free oxime with (B) a metal cyanide (e.g. sodium cyanide) in the presence of (C) about 1.0-1.3 equivalent of sodium carbonate and/or sodium hydroxide based on 1 equivalent of the acid component of the alpha-chloroxime salt. EFFECT:The reaction proceeds by using only about stoichiometric amount of metal cyanide. There is not generation of hydrogen cyanide and the objective compound can be produced in high yield.

    PRODUCTION OF HIGH-PURITY N-(CYCLOHEXYLTHIO)-PHTAHLIMIDE
    27.
    发明专利
    PRODUCTION OF HIGH-PURITY N-(CYCLOHEXYLTHIO)-PHTAHLIMIDE 失效

    公开(公告)号：JPS61212560A

    公开(公告)日：1986-09-20

    申请号：JP5254485

    申请日：1985-03-18

    Applicant: TORAY INDUSTRIES

    Inventor： ONO TAKAE ,  MATSUKUMA YOSHIHISA

    IPC: C07D209/48

    Abstract: PURPOSE:To obtain the titled substance, by reacting phthalimide with cyclohexylsulfenyl chloride in the presence of an alkali (earth) metallic hydroxide and an organic solvent, blending the reaction product with an organic amine, neutralizing the organic amine, separating the solution and crystallizing the titled substance from the organic solvent layer. CONSTITUTION:Phthalimide is reacted with cyclohexylsulfenyl chloride in the presence of an alkali (earth) metallic hydroxide and an organic solvent, the reaction product is blended with an organic amine (e.g., triethylamine) at 60-120 deg.C, the organic amine is treated with a mineral acid (e.g., aqueous solution of hydrochloric acid), transferred as a mineral acid salt into the water layer, the organic solvent layer is separated, and the aimed high-purity substance is obtained by crystallization from the organic solvent layer. EFFECT:The aimed substance having >=99% high purity is obtained. USE:An inhibitor against early vulcanization of naturally occurring or synthetic rubber.

    PRODUCTION OF HIGH-PURITY N-(CYCLOHEXYLTHIO)-PHTHALIMIDE
    28.
    发明专利
    PRODUCTION OF HIGH-PURITY N-(CYCLOHEXYLTHIO)-PHTHALIMIDE 失效

    公开(公告)号：JPS61212559A

    公开(公告)日：1986-09-20

    申请号：JP5254385

    申请日：1985-03-18

    Applicant: TORAY INDUSTRIES

    Inventor： ONO TAKAE ,  MATSUKUMA YOSHIHISA

    IPC: C07D209/48

    Abstract: PURPOSE:To obtain the titled substance, by reacting phthalimide with cyclohexylsulfenyl chloride in the presence of an organic amine and an organic solvent, neutralizing the organic amine with a mineral acid, blending the organic solvent layer with an alkali aqueous solution, and crystallizing the titled substance from the organic layer. CONSTITUTION:Phthalimide is reacted with cyclohexylsulfenyl chloride in the presence of an organic amine (preferably triethylamine) and an organic solvent (e.g., CCl4), the organic amine in the formed reaction solution is neutralized with a mineral acid (e.g., 3wt% aqueous solution of hydrochloric acid), transferred as a mineral acid salt into the water layer. On the other hand, the organic solvent layer is blended with an alkali aqueous solution (e.g., aqueous solution of NaOH), unreacted phthalimide and impurities are transferred into the aqueous solution, and the aimed substance is crystallized from the organic solvent layer. The temperature of the alkali aqueous solution during in blending is preferably room temperature to avoid decomposition of the aimed substance. EFFECT:>=99.5wt% purity is possible. USE:An inhibitor against early vulcanization of naturally occurring or synthetic rubber.

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