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    5-CARBAMOYLFLUOROMETHYLIDENE HYDANTOIN COMPOUND AND ITS PREPARATION
    53.
    发明专利
    5-CARBAMOYLFLUOROMETHYLIDENE HYDANTOIN COMPOUND AND ITS PREPARATION 失效

    公开(公告)号：JPS60181073A

    公开(公告)日：1985-09-14

    申请号：JP3535884

    申请日：1984-02-28

    Applicant: UBE INDUSTRIES

    Inventor： FUKUI KIYOSHI ,  KAKEYA NOBORU ,  MATSUO FUMIO

    IPC: C07D233/96

    Abstract: NEW MATERIAL:The 5-carbamoylfluoromethylidenehydantoin of formula I (R is H, alkyl or allyl). EXAMPLE:5-Carbamoylfluoromethylidenehydantoin. USE:Pharmaceuticals, agricultural chemicals or their raw materials. PREPARATION:The compound of formula I can be prepared by reacting 1mol of 5-(alkyoxycarbonyl)fluoromethylidenehydantoin of formula II (R is lower alkyl) with 3-20mol of the amine of formula R -NH2 such as ammonia, methylamine, etc. in the presence of water at room temperature for

    PREPARATION OF TERTIARY DICHLOROPHOSPHINE
    56.
    发明专利
    PREPARATION OF TERTIARY DICHLOROPHOSPHINE 失效

    公开(公告)号：JPS55164693A

    公开(公告)日：1980-12-22

    申请号：JP7306279

    申请日：1979-06-12

    Applicant: UBE INDUSTRIES

    Inventor： FUKUI KIYOSHI ,  KAKEYA NOBORU ,  SUGIHARA HIROSHI

    IPC: C07F9/535

    Abstract: PURPOSE:To obtain the titled compound with ease in short period of time in high yields useful as a raw material for tertiary phosphine, etc. by reacting a tertiary phosphine prepared by various organic synthetic reactions as by-products with Cl2 and CO. CONSTITUTION:A tertiary phosphine sulfide shown by the formula I (R is 1-18C alkyl, 6-14C aryl, the three R may be the same or different) is reacted with Cl2 and CO to give a tertiary dichlorophospine shown by the formula II. The reaction is carried out in a solvent, e.g. CCl4, et. at -20-250 deg.C. CO is preferably fed by a feed pressure of 3-100kg/cm . Tertiary phosphine sulfides prepared using tertiary phosphines as a desulfurizing agent can be used as a raw material. A prepared compound shown by the formula II can be converted with ease into tertiary phosphines or tertiary phosphineimines.

    PREPARATION OF TERTIARY DICHLOROPHOSPHINE
    57.
    发明专利
    PREPARATION OF TERTIARY DICHLOROPHOSPHINE 失效

    公开(公告)号：JPS55164692A

    公开(公告)日：1980-12-22

    申请号：JP7305979

    申请日：1979-06-12

    Applicant: UBE INDUSTRIES

    Inventor： FUKUI KIYOSHI ,  KAKEYA NOBORU ,  SUGIHARA HIROSHI

    IPC: C07B47/00 ,  C07B31/00 ,  C07C67/00 ,  C07F9/535

    Abstract: PURPOSE:To obtain the titled compound in high yields useful as a raw material for a tertiary phosphine through one step reaction requiring no catalyst, by reacting a tertiary phosphine sulfide prepared as by-products in organic synthetic reactions with phosgene. CONSTITUTION:A tertiary phosphine sulfide shown by the formula I (R is 1-18C alkyl, 6-14C aryl, the three R may be the same or different) is reacted with phosgene to give a tertiary dichlorophosphine shown by the formula II. The reaction is carried out preferably in a solvent, e.g., acetonitrile, at -20-250 deg.C. Tertiary phosphine sulfide prepared as a by-product in using tertiary phosphine as a desulfurizing agent can be used for a raw material. The obtained compound shown by the formula 2 can be converted easily into a tertiary phosphine or a tertiary phosphineimine.

    PREPARATION OF TRIPHENYLPHOSPHINE
    58.
    发明专利
    PREPARATION OF TRIPHENYLPHOSPHINE 失效

    公开(公告)号：JPS55149294A

    公开(公告)日：1980-11-20

    申请号：JP5700979

    申请日：1979-05-11

    Applicant: UBE INDUSTRIES

    Inventor： FUKUI KIYOSHI ,  KAKEYA NOBORU

    IPC: C07F9/50 ,  C07F9/535

    Abstract: PURPOSE:To obtain the titled compound useful as a reducing agent for the synthesis of organic compounds and as a disoxidant for nitro compounds in high yield, by reacting a triphenylphosphine dihalogenide with hydrogen in a specific solvent under pressure. CONSTITUTION:A triphenylphosphine dihalogenide (P) is reacted with hydrogen in a solvent, e.g. chlorobenzene and/or dichlorobenzene, under pressure at 100-250 deg.C to give triphenylphosphine. The amount of the solvent is 5-50pts.wt. per pts.wt. of (P). Preferably, (P) is brought into contact with hydrogen in the presence of an oxygen- contaning gas, e.g. air, at a partial pressure of hydrogen of 1.5-50kg/cm .

    PREPARATION OF TERTIARY PHOSPHINE
    59.
    发明专利
    PREPARATION OF TERTIARY PHOSPHINE 失效

    公开(公告)号：JPS55149293A

    公开(公告)日：1980-11-20

    申请号：JP5700879

    申请日：1979-05-11

    Applicant: UBE INDUSTRIES

    Inventor： FUKUI KIYOSHI ,  KAKEYA NOBORU ,  KITA JIYUNICHIROU ,  FUJIMURA SUSUMU

    IPC: C07F9/50 ,  B01J27/00 ,  B01J27/06 ,  B01J31/00 ,  B01J31/16 ,  C07B61/00

    Abstract: PURPOSE:To obtain the titled compound useful as a reducing agent for the synthesis of organic compounds and as a disoxidant for nitro compounds in high yield, by reacting phosphine dihalogenide with hydrogen in the presence of a specific compound of a platinum group metal. CONSTITUTION:A compound of formula I (R is 1-18C alkyl or 6-14C aryl group; X is Cl, Br, I, etc.), e.g. trimethylphosphine dihalogenide, is reacted with hydrogen in the presence of one or more compounds selected from the group consisting of a halide of a platinum group metal, e.g. rhodium chloride, and a platinum group metal complex, e.g. dichlorobis (triphenylphosphine)palladium (II), at 100-250 deg.C to give a tertiary phosphine of formula II. For example, triphenylphosphine is obtained in 93% yield, using RhCl3 as a catalyst. EFFECT:A short reaction time even under a low pressure as low as 10kg/cm .

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