Methyl-heptenone prepn. from methyl-hydroxy-heptanone - by heating with acid catalysts while preventing escape of reaction intermediate

    公开(公告)号:DE2641268A1

    公开(公告)日:1978-03-16

    申请号:DE2641268

    申请日:1976-09-14

    Applicant: BASF AG

    Abstract: Prepn. of 2-Me-1- and 2-Me-2-hepten-6-one (Ia and Ib) comprises heating 2-Me-heptan-2-ol-6-one, (II), or residues contg. (II), to 80-300 degrees C in the presence of strongly acid catalysts. The escape of 2,2,6-trimethyl-2,3-dihydro-4H-pyran, (III), formed as intermediate, from reaction mixt. is prevented, by working in a closed system under press. of reactants or pref. by using a reaction vessel fitted with a reflux condenser and a phase sepn. vessel. Vapour mixt. of (III) and H2O is condensed; H2O is removed and (III)-rich upper phase is recycled to reactor. (I) are intermediates for synthesis of carotinoids and perfumes, e.g. isophytol and ionone.

    (1)-Alkyl-allyl ester prodn. - by isomerisation of (3)-alkyl-allyl ester in presence of copper carboxylic acid and anhydride

    公开(公告)号:DE2611664A1

    公开(公告)日:1977-09-29

    申请号:DE2611664

    申请日:1976-03-19

    Applicant: BASF AG

    Abstract: Prodn. of allyl esters (I) of the formula CH2=CH-CHR'-O-CO-R" (in which R' is 1-4C alkyl, opt. with an acyloxy substit. with max. 4C. alkyl or H) involves isomerisation of allyl esters (II) of the formula R'-CH=CH-CH2-O-CO-R" at elevated temp., as in DT 2406058, in the presence of Cu and/or Cu (I) or Cu (II) cpds. and in the presence of carboxylic acids (III). The improvement comprises the use of carbocylic anhydride (IV) in addn. to (III). (IV) pref. is the anhydride of (III), esp. acetic anhydride (IVa), and is used in an amt. of 0.1-10 mole-% wrt (III). In an example but-2-en-1,4-diyl acetate was isomerise to but-2-en-3,4-diyl acetate in the presence of (IVa) the yield being 10% and amt. of by-prods. 1%. If (IVa) was omitted, the yield was up to 2.5% and amt of by-prods. 1.5%. (I) are used as starting materials in organic syntheses.

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