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    11AMINOO22SUBSTITUTEDD1*22DIETHOXYCARBONYL ETHYLENE
    31.
    发明专利
    11AMINOO22SUBSTITUTEDD1*22DIETHOXYCARBONYL ETHYLENE 失效

    公开(公告)号：JPS56103143A

    公开(公告)日：1981-08-18

    申请号：JP528980

    申请日：1980-01-22

    Applicant: UBE INDUSTRIES

    Inventor： FUKUI KIYOSHI ,  KITA JIYUNICHIROU ,  KAKEYA NOBORU ,  FUJIMURA SUSUMU ,  OKIMOTO KIYOMI ,  JIBIKI HIROSHI

    IPC: C07C229/30 ,  C07C229/36

    Abstract: NEW MATERIAL:The titled compound of formula I (Y is benzoyl, acetyl or ethoxycarbonyl). EXAMPLE:1-Amino-2-benzoyl-1,2-diethoxycarbonyl ethylene. USE:Intermediate of pharmaceuticals, pesticides, polymer additives, etc. For example, the reaction of the compound with an isocyanate compound affords a hydantoic derivative having herbicidal and fungicidal activities. PROCESS:The compound of formula I is prepared by (1) reacting ethyl cyanoformate with an active methylene compound of formula II (e.g. ethyl benzoylacetate, ethyl acetoacetate, etc.) in the presence of a metal halide of formula MX4 (M is Ti or Sn; X is F, Cl, Br, etc.) under anhydrous conditions in a solvent such as benzene, toluene, etc. pref. at -10-+100 deg.C, and (2) treating the reaction product with water or an acidic aqueous solution.

    PREPARATION OF AMINO ACID ESTER
    32.
    发明专利
    PREPARATION OF AMINO ACID ESTER 失效

    公开(公告)号：JPS5687542A

    公开(公告)日：1981-07-16

    申请号：JP16402379

    申请日：1979-12-19

    Applicant: UBE INDUSTRIES

    Inventor： FUKUI KIYOSHI ,  KITA JIYUNICHIROU ,  JIBIKI HIROSHI ,  KAKEYA NOBORU ,  FUJIMURA SUSUMU ,  OKIMOTO KIYOMI

    IPC: C07B61/00 ,  B01J23/06

    Abstract: PURPOSE:To obtain the titled compound, useful as an intermediate of pharmaceuticals, agricultural chemicals, etc., without using a base, by the reaction of a cyanoformate and a halo (active methylene) compound in the presence of Zn followed by treatment with water or an acidic aqueous solution. CONSTITUTION:A compound of formula I (R is 1-4C alkyl) and a compound of formula II [X is Cl or Br; R is 1-4C alkyl; Y is CN, COR (R3 is 1-4C alkyl or 6-14C aryl), or COOR (R is 1-4C alkyl)] are made to react in a solvent (e.g. benzene, THF etc.) or in the absence of a solvent at 50-100 deg.C in the presence of Zn (preferably Zn activated with Cu). The product obtained is treated with water or an acidic aqueous solution (e.g. hydrochloric acid, sulfuric acid, etc.) at 0-35 deg.C to give a compound of formula III (e.g. 1-amino-2-cyano-1,2-dimethoxycarbonylethylene).

    PREPARATION OF AMINO ACID ESTER
    33.
    发明专利
    PREPARATION OF AMINO ACID ESTER 失效

    公开(公告)号：JPS5671050A

    公开(公告)日：1981-06-13

    申请号：JP14777879

    申请日：1979-11-16

    Applicant: UBE INDUSTRIES

    Inventor： FUKUI KIYOSHI ,  OKIMOTO KIYOMI ,  KITA JIYUNICHIROU ,  SUGIHARA HIROSHI ,  FUJIMURA SUSUMU ,  KAKEYA NOBORU

    IPC: C07B61/00

    Abstract: PURPOSE:To obtain the titled compound which is a synthetic intermediate for additives of medicines, agricultural chemicals and high polymers readily in high yield, by reacting a cyanoformate with an active methylene compound in the presence of a metal halide. CONSTITUTION:A cyanoformate of formula I (R is 1-4C alkyl), e.g. methyl cyanoformate of butyl cyanoformate, is reacted with an active methylene compound of formula II (R is 1-4C alkyl: Y is group of CN, etc.), e.g. methyl cyanoacetate or propyl cyanoacetate, in the presence of a metal halide of the formula MXn (M is titanium or tin; X is F, Cl, Br or I; n is the same number as the miximum valence of M), e.g. titanium tetrachloride or stannic chloride, and the resultant reaction product is then treated with water or an acidic aqueous solution to give the titled compound of formula III in high yield without using a base.

    PREPARATION OF HEXAMETHYLENEIMINES
    35.
    发明专利
    PREPARATION OF HEXAMETHYLENEIMINES 失效

    公开(公告)号：JPS5337682A

    公开(公告)日：1978-04-06

    申请号：JP11073376

    申请日：1976-09-17

    Applicant: UBE INDUSTRIES

    Inventor： MAZAKI MITSUO ,  KITA JIYUNICHIROU

    IPC: C07D295/02 ,  C07D223/04

    Abstract: PURPOSE:To prepare hexamethyleneimines useful as intermediate for phamaceuticals and pesticides, and also useful for corrosinproof agents for metals, textile softeners, and rubber additives, in high yield by catalytic hydrogenation of 2-amino-2H-azepines with hydrogen.

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