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    54.
    发明专利
    未知

    公开(公告)号：DE19852691A1

    公开(公告)日：2000-05-18

    申请号：DE19852691

    申请日：1998-11-16

    Applicant: BASF AG

    Inventor： OOST CARSTEN ,  STROEZEL MANFRED ,  ETZRODT HEINZ ,  WELLER DIETMAR ,  RHEUDE UDO ,  KAIBEL GERD ,  KRUG THOMAS ,  SPISKE LUISE ,  JAEDICKE HAGEN

    IPC: B01J31/14 ,  C07B61/00 ,  C07C45/67 ,  C07C45/74 ,  C07C49/203

    Abstract: Preparation of unsaturated ketones by reaction of the corresponding alpha , beta -unsaturated alcohol with an alkyl acetoacetate compound in the presence an organo-aluminum catalyst at constant temperature, with separation and continuous removal of CO2 and alcohol formed. Preparation of unsaturated ketones of formula (I) by reaction of the corresponding alpha , beta -unsaturated alcohol of formula (II) with an alkyl acetoacetate compound of formula (III) in the presence of 0.1-5 mole% (based on (III)) of an organo-aluminum catalyst with separation and continuous distillative removal of CO2 and alcohol of formula R3OH formed during reaction, in a reactor containing a fractionation column, where: (A) (II) is added to the reaction mixture together with the organic catalyst without additional solvent and (III) is then added to this mixture; (B) the reaction temperature is kept constant between 175-220 degrees C; (C) the content of (III) is kept at a constant level between 0.1-10 wt.% during the reaction. R1, R3 = 1-4C alkyl; R2 = 4-30C aliphatic, cycloaliphatic or cycloaliphatic-aliphatic; a, b = optional additional bonds.

    Unsaturated ketone preparation by modified Carroll reaction
    55.
    发明专利
    Unsaturated ketone preparation by modified Carroll reaction 未知

    公开(公告)号：DE19815810A1

    公开(公告)日：1999-10-14

    申请号：DE19815810

    申请日：1998-04-08

    Applicant: BASF AG

    Inventor： OOST CARSTEN ,  STROEZEL MANFRED ,  ETZRODT HEINZ ,  BOCKSTIEGEL BERNHARD ,  JAEDICKE HAGEN

    IPC: B01J31/02 ,  B01J31/14 ,  C07C45/67 ,  C07F5/06 ,  C07C49/20 ,  C07C29/68 ,  C07C31/32 ,  C07C45/68

    Abstract: Preparation of psi , delta -unsaturated ketones (I) by modified Carroll reaction is catalysed by a stable liquid aluminum acetoacetate compound or mixture of such compounds. Some such catalyst mixtures are new. Preparation of psi , delta -unsaturated ketones of formula (I) involves modified Carroll reaction of an allyl alcohol of formula (II) with diketene or an alkyl acetoacetate of formula (III) in presence of an aluminum catalyst. R1 = H or 1-20C, saturated or unsaturated, branched hydrocarbyl; R2 = 1-5C alkyl. The novelty is that the catalyst consists of an aluminum compound (or aluminum compound mixture) which is a stable liquid at room temperature and contains at least one alkyl acetoacetate-forming group and 1 or 2 alkoxy groups or exclusively alkyl acetoacetate forming groups which are esterified sec. butanol or isobutanol or with at least two different alkanols. Independent claims are included for: (1) new mixtures of aluminum tris-acetoacetates of formula (V) which are liquid at room temperature; and (2) the preparation of mixtures as in (1). R3 = 1-5C alkyl, preferably Me or Et; R4 = 3-10C alkyl, preferably CHMe2, CH(Me)Et, CMe3 or CH(Me)-C3H7; R5 = 1-10C alkyl, preferably Me, Et, CHMe2, CH(Me)Et or CH(Me)-C3H7; provided that R3-R5 are not all the same. A further Independent claim relates to the continuous preparation of compounds (V) (or their mixtures), having the narrower proviso that R3-R5 can only be the same if they are -CH(Me)Et or -CH2CHMe2, which are liquid at room temperature. The process involves continuously reacting 1 mole of aluminum alcoholate of formula (VI) with 3-10 moles of (III), or with at least 3 moles of a mixture of 2 or 3 different compounds (III), optionally dissolved in an inert solvent. Reaction is at 100-250 (preferably 150-200) deg C and 1-100 (preferably 1-10) bars with a dwell time of 5-120 (preferably 15-45) minutes, the pressure and temperature being such that no gas phase is formed in the reaction vessel. R6 = 2-10C alkyl, preferably -CH2CHMe2, -CH(Me)Et or -CH(Me)C3H7; provided that R2 and R6 can only be the same if they are -CH(Me)Et or -CH2CHMe2.

    58.
    发明专利
    未知

    公开(公告)号：DE3302498A1

    公开(公告)日：1984-07-26

    申请号：DE3302498

    申请日：1983-01-26

    Applicant: BASF AG

    Inventor： LAAS HARALD DR ,  TAVS PETER DR ,  HANNEBAUM HEINZ ,  STROEZEL MANFRED

    IPC: C07C46/08 ,  C07F15/06 ,  C07C119/10 ,  C07C50/02

    Abstract: Improved process for the preparation of salcomine useful as an oxidation catalyst for the oxidation of alkylated phenols to the corresponding alkylated p-benzoquinones by reacting salicylaldehyde with ethylenediamine in a mole ratio of about 2:1 and a cobalt salt in a liquid reaction medium wherein the reaction medium is a linear or cyclic carboxamide which is disubstituted on the nitrogen, in particular dimethylformamide, and the cobalt salt is cobalt carbonate or with the cobalt hyroxide carbonate, 2 CoCO3.3 Co(OH)2.H2O. Preparation of the salcomine in accordance with the invention offers significant advantages, both in the preparation of the salcomine itself and in the subsequent oxidation of the trimethylphenol to trimethyl-p-benzoquinone utilizing the salcomine.

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