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    Production of Alpha, Omega-diaminoalkane Carboxylic Acids
    118.
    发明专利
    Production of Alpha, Omega-diaminoalkane Carboxylic Acids 未知

    公开(公告)号：GB1153275A

    公开(公告)日：1969-05-29

    申请号：GB4370466

    申请日：1966-09-30

    Applicant: BASF AG

    Inventor： KOENIG KARL-HEINZ ,  POMMER HORST

    IPC: C07C227/08

    Abstract: 1,153,275. Production of diamino carboxylic acids. BADISCHE ANILIN- & SODA-FABRIK A.G. 30 Sept., 1966 [1 Oct., 1965], No. 43704/66. Heading C2C. α,#-Diaminoalkane carboxylic acids are obtained by reacting an a, co-dihaloalkanoic acid or an alkali metal, ammonium or alkaline earth metal salt thereof with hexamethylene tetramine in aqueous medium at pH 3 to 11 at -10‹ C. to 70‹ C. when the pH is above 9 or at - 10‹ C. to 130‹ C. when the pH is not more than 9. The reaction may be effected in two stages and the intermediates formed, i.e. aminohaloalkanoic acids or the hexamethylene tetramine adducts thereof, may be isolated. The hexamethylene tetramine may be replaced by a mixture of aqueous formaldehyde and ammonia and in this case more ammonia is suitably added as the reaction proceeds. The reaction may be catalysed by the addition of alkali metal, alkaline earth metal ammonium or amine halides.

    Halo-substituted epsilon caprolactones
    119.
    发明专利
    Halo-substituted epsilon caprolactones 未知

    公开(公告)号：GB1135067A

    公开(公告)日：1968-11-27

    申请号：GB1192066

    申请日：1966-03-18

    Applicant: BASF AG

    Inventor： KOENIG KARL-HEINZ ,  POMMER HORST

    IPC: C07D313/04 ,  C08G63/682

    Abstract: 1,135,067. Halo - 6 - hydroxy - hexanolactones. BADISCHE ANILIN- & SODAFABRIK A.G. 18 March, 1966 [20 March, 1965], No. 11920/66. Heading C2C. 3-Halo- and 4-halo-6-hydroxyhexanolactones (i.e. 6-hydroxycaprolactones) and the preparation thereof wherein a 3,6-dihalohexanoic acid and/or a 4,6-dihalohexanoic acid is either (a) heated in the absence of water, optionally in the presence of a specified inert solvent (e.g. an aromatic hydrocarbon) to a temperature of 120‹ to 280‹ C.; (b) treated at - 10‹ to 120‹ C. with water alone or with an aqueous acid (e.g. a non-oxidizing inorganic acid or a low molecular weight aliphatic carboxylic acid); or (c) treated at - 10‹ to 50‹ C. with an aqueous alkali (e.g. an alkali metal or alkaline earth metal oxide, hydroxide, carbonate or alcoholate or a specified organic base; water being added thereafter in case (a), and the reaction mixture being brought to a pH value of 1 to 4 and heated for at least a short time to 70‹ to 150‹ C. at this pH value in case (c), and the desired 6-hydroxyhexanolactones then being isolated by conventional means, e.g. by adjusting the pH of the reaction mixture to 4À5 to 7 and extracting with an organic solvent for the lactones. The above process may also be effected by heating the starting materials with an aqueous solution of an alkali metal or alkaline earth metal halide derived from a halogen having a higher atomic weight than the halogen in the 6-position of the said starting materials. According to a further embodiment of the invention a mixture containing a 6- monohalohexanoic acid in addition to the 4,6- and/or 3,6-dihalohexanoic acids is reacted with water to give a mixture of the 3- and/or 4- halocaprolactone and halohexanoic acid which is extracted with an organic water-immiscible solvent, and the 3- and/or 4-halocaprolactone is recovered from the extract and the unchanged 6-halohexanoic acid from the aqueous layer. Numerous suitable starting materials are specified and the preparation of 3- and 4-chloro- and 3- and 4-bromo-substituted 6-hydroxyhexanolactones is described..

    Separating tertiary phosphines from olefinic compounds
    120.
    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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