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    PRODUCTION OF SOLID DISODIUM P-HYDROXYBENZOATE
    8.
    发明专利
    PRODUCTION OF SOLID DISODIUM P-HYDROXYBENZOATE 失效

    公开(公告)号：JPS62258340A

    公开(公告)日：1987-11-10

    申请号：JP9959786

    申请日：1986-04-30

    申请人： NIPPON PETROCHEMICALS CO LTD

    发明人： TANIMOTO FUMIO ,  KITANO HISAO

    IPC分类号： C07C65/03 ,  B01J23/00 ,  B01J23/72 ,  C07B61/00 ,  C07C51/00 ,  C07C51/093 ,  C07C67/00

    摘要： PURPOSE:To efficiently obtain the titled compound in good yield, by reacting phenol with CCl4 and NaOH in amounts of specific proportions in the presence of a specific amount of transition metal powder catalyst in a specific aqueous solution, cooling the reaction mixture to a specific temperature and separating the titled compound. CONSTITUTION:CCl4 in an amount of 0.9-1.2mol based on 1mol phenol and NaOH in an amount of 7-20mol based on 1mol phenol are present in an aqueous solution containing disodium p-hydroxybenzoate and/or sodium chloride in an amount of 10-40wt% in the initial period of reaction in the presence of a transition metal powder, preferably copper powder, etc., in an amount of 0.01-1.00wt% based on the reaction system, as necessary, in the coexistence of a surfactant or solubilizing agent to carry out reaction at 50-150 deg.C. The resultant reaction mixture is then cooled to -20-+20 deg.C to separate and afford the aimed compound. EFFECT:Since the reaction system is not neutralized after completing the reaction, NaOH in an excess amount can be effectively recovered and reused and the formation of by-products can be suppressed by maintaining the reaction raw material ratio at a constant value.

    ESTER HAVING SUBSTITUTED NORBORNYL GROUP AND PERFUME COMPOSITION CONTAINING SAID ESTER
    9.
    发明专利
    ESTER HAVING SUBSTITUTED NORBORNYL GROUP AND PERFUME COMPOSITION CONTAINING SAID ESTER 失效

    公开(公告)号：JPS62149643A

    公开(公告)日：1987-07-03

    申请号：JP29566685

    申请日：1985-12-25

    申请人： NIPPON PETROCHEMICALS CO LTD

    发明人： INOUE YOSHIHARU ,  TANIMOTO FUMIO ,  KITANO HISAO

    IPC分类号： C11D3/50 ,  A61K8/37 ,  A61Q13/00 ,  C07C69/06 ,  C07C69/614 ,  C07C69/618 ,  C07C69/78 ,  C11B9/00 ,  C11D9/44

    摘要： NEW MATERIAL:A compound expressed by formula I (C2 is ethyl, vinyl or ethylidene substituted at the 5- or 6-position of the norbornane ring; R1 is 1-3C alkyl; R2 is carboxylic acid residue derived from acetic acid, benzoic acid, phenylacetic acid and cinnamic acid; the dotted line in the side chain constituting the ester indicates that the C-C bond is single or double bond). EXAMPLE:1-(5- or 6-Vinylnorbornan-2-yl)-2-methyl-3-acetoxy-1-pentene. USE:One component in perfume compositions, having improved fragrance, e.g. woody fragrance, floral woody fragrance, etc., and usable for perfume, hair dressing, interior perfume, deodorant, insecticide, soap, toiletry, etc. PREPARATION:An alcohol expressed by formula II is reacted and esterified with a chloride of a carboxylic acid, e.g. acetyl chloride, etc., or carboxylic acid, e.g. cinnamic acid, etc., in a solvent to afford the aimed compound expressed by formula I.

    ETHYLNORBORNYL-2-ALDEHYDE AND ITS PREPARATION
    10.
    发明专利
    ETHYLNORBORNYL-2-ALDEHYDE AND ITS PREPARATION 失效

    公开(公告)号：JPS5832841A

    公开(公告)日：1983-02-25

    申请号：JP13174381

    申请日：1981-08-22

    申请人： NIPPON PETROCHEMICALS CO LTD

    发明人： INOUE YOSHIHARU ,  TANIMOTO FUMIO ,  KITANO HISAO

    IPC分类号： C07C45/50 ,  B01J23/00 ,  B01J23/46 ,  B01J31/00 ,  B01J31/20 ,  C07C45/00 ,  C07C45/58 ,  C07C47/347 ,  C07C67/00

    摘要： NEW MATERIAL:The compound of formulaI(C2H5 is bonded to the 5- or 6- position of norbornane ring; R1 and R2 are H or CH3). EXAMPLE:5- or 6-Ethylnorbornyl-2-aldehyde. USE:Raw material of perfumery, reagent for organic syntheses, raw material of polymer, etc. PROCESS:(A) The compound of formulaI(R1 and R2 are especially H) can be prepared by hydrolyzing the compound of formula II (R3 is 1-6C hydrocarbon group; R1 and R2 are especially H), and decarbonating the product at 0-250 deg.C. (B) Another compound of formulaI(R2 is H) can be prepared by reacting the compound of formula III with carbon monoxide and hydrogen in the presence of a catalyst consisting preferably of a compound of a 8-group element of the periodic table, especially a compound of Co, Rh, Ir, Ru or Pt, at 30-300 deg.C. (C) As an alternative method, the compound of formulaIis obtained by the partial hydrogenation of the compound of formula IV[C2 is vinyl (the dotted line is single bond) or ethylidene (the dotted line is double bond)].