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    Production of axerophthyl phosphonium salts
    21.
    发明专利
    Production of axerophthyl phosphonium salts 未知

    公开(公告)号：GB969180A

    公开(公告)日：1964-09-09

    申请号：GB1965863

    申请日：1963-05-17

    Applicant: BASF AG

    Inventor： SARNECKI WILHELM ,  NUERRENBACH AXEL ,  REIF WERNER

    IPC: C07F9/54

    Abstract: Quaternary axerophthyl phosphonium salts are prepared by reacting an ester of vitamin A alcohol (axerophthol) with a tertiary phosphine and an acid or with acid addition salts of tertiary phosphines A solvent may be used. Preferred temperatures are from 0-80 DEG C., but -20 to +120 DEG C. may be used. The initial material may be a waste liquor containing a vitamin A ester obtained in the production and purification of vitamin A esters. Specified phosphines are triphenyl, tri-p-tolyl and trianisyl phosphines. Suitable acids include sulphuric acid, organic sulphonic acids and fluorboric acid. Specified vitamin A esters are the acetate, propionate and palmitate. The vitamin A esters may be in the cis- or trans-form. Specification 812,522 is referred to.

    FORMULATION OF VITAMIN A ESTERS
    23.
    发明专利
    FORMULATION OF VITAMIN A ESTERS 未知

    公开(公告)号：GB1300658A

    公开(公告)日：1972-12-20

    申请号：GB1980370

    申请日：1970-04-24

    Applicant: BASF AG

    Inventor： REIF WERNER ,  NUERRENBACH AXEL ,  FRETSCHLAG HERWIG

    IPC: A61K31/07 ,  A61K47/44 ,  C07C403/00

    Abstract: 1300658 Vitamin A esters BADISCHE ANILIN. & SODA-FABRIK AG 24 April 1970 19803/70 Heading C2V [Also in Division A5] Vitamin A esters in a stable form are obtained by dispersing them in organic liquids in which the esters are more soluble at elevated temperature than at room temperature, the mean particle sizes of the esters being from 10 to 400 microns. Preferably at least 25% of the ester is present in dispersed form at room temperature and a clear solution is obtained when heated to 60‹ to 80‹ C. to enable the ester to be accurately dispensed. In examples Vitamin A acetate is dispersed in peanut oil and in heptane.

    Separating tertiary phosphines from olefinic compounds
    27.
    发明专利
    Separating tertiary phosphines from olefinic compounds 未知

    公开(公告)号：GB1100250A

    公开(公告)日：1968-01-24

    申请号：GB3810166

    申请日：1966-08-25

    Applicant: BASF AG

    Inventor： REIF WERNER ,  HAUG PETER ,  FREYSCHLAG HERWIG ,  POMMER HORST

    IPC: C07C11/00 ,  C07C403/00

    Abstract: Olefinic compounds of formula where R4, R5, R6 and R7 are hydrogen atoms or saturated or unsaturated aliphatic, cycloaliphatic, araliphatic or aromatic radicals, the total number of carbon atoms being at least eight, and in which radicals R4 and R5 and/or R6 and R7 may form a fiveto eight-membered ring, said compounds being contaminated by tertiary phosphines of formula where R1, R2 and R3 are aliphatic, cycloaliphatic, araliphatic or aromatic hydrocarbon radicals having one to eight carbon atoms, are purified by contacting water-insoluble organic solutions of the olefinic compounds with aqueous solutions of peroxides or with redox resins bearing peroxide groups to convert the phosphines to tertiary phosphine oxides of formula and then separating the tertiary phosphine oxides, e.g. by extraction with suitable solvents. Olefinic compounds which may be purified include axerophthene and lycopene.ALSO:Olefinic compounds of formula where R4, R5, R6 and R7 are hydrogen atoms or saturated or unsaturated aliphatic, cyclo-aliphatic, araliphatic or aromatic radicals which may contain ester, ether, nitrile, carbonyl or hydroxyl groups, the total number of carbon atoms being at least eight, and in which radicals R4 and R5 and/or R6 and R7 may form a fiveto eight-membered ring, said compounds being contaminated by tertiary phosphines of formula where R1, R2 and R3 are aliphatic, cycloaliphatic, araliphatic or aromatic hydrocarbon radicals having one to eight carbon atoms, are purified by contacting water-insoluble organic solutions of the olefinic compounds with aqueous solutions of peroxides or with redox resins bearing peroxide groups to convert the phosphines to tertiary phosphine oxides of formula and then separating the teritary phosphine oxides, e.g. by extraction with suitable solvents. In examples, Vitamin A acid ethyl ester, Vitamin A acetate and Vitamin A palmitate, all containing triphenyl phosphine, are dissolved in octane, cyclohexane and light naphtha, and contacted with aqueous solutions of potassium hydrogen permonosulphate, hydrogen peroxide and permonosulphuric acid and with a peroxide redox resin, the phosphine oxides then being removed by extraction with mixtures of methanol and water and ethanol and water. Other olefinic compounds which may be purified are linalool, dehydrolinalool, a -ionone, b -ionone, Vitamin A aldehyde, Vitamin A2 acetate, Vitamin A2 acid ethyl ester, axeropthene, b - apo - 121 - carotenal, b - apo-121-carotenal acetate, b -apo-121-carotenic acid ethyl ester, b -apo-81-carotenal, b -apo-81-caro-tenal acetate, b -apo-81-carotenic acid ethyl ester, a -carotene, b -carotene, lycopene, farnesylacetone and isophytol.

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