Method for the production of trioxime derivatives
    13.
    发明授权
    Method for the production of trioxime derivatives 失效
    生产三肟衍生物的方法

    公开(公告)号:US06906223B2

    公开(公告)日:2005-06-14

    申请号:US10332046

    申请日:2001-07-04

    CPC classification number: C07C249/06 C07C249/08 C07C251/40

    Abstract: The present invention relates to a process for preparing trioxime derivatives of the formula I in which the substituents R1 and R2 are identical or different and each is cyano, alkyl, haloalkyl or cycloalkyl, and R3 and R4 are identical or different and each is alkyl, haloalkyl, cycloalkyl, alkylcarbonyl or arylalkyl, by the following reaction steps in water without isolation of the intermediates: A) nitrosation of 1,3-diketones of the formula II  to give monooximes of the formula III, B) oximation of III with hydroxylamine derivatives of the formula IV H2N—OR3′  IV  in which R3′ is hydrogen or a group R3 to give bisoximes of the formula V, C) alkylation of V with alkylating agents or acylation of V with acylating agents to give compounds of the formula VI and D) subsequent oximation of VI with hydroxylamine to give compounds of the formula I.

    Abstract translation: 本发明涉及一种制备式I的三肟衍生物的方法,其中取代基R 1和R 2是相同或不同的,并且各自为氰基,烷基,卤代烷基 或环烷基,R 3和R 4相同或不同,并且各自为烷基,卤代烷基,环烷基,烷基羰基或芳烷基,通过以下反应步骤在水中不分离 中间体:A)式II的1,3-二酮的亚硝化,得到式III的单肟,B)III式与Ⅳ的羟胺衍生物的肟化,其中式Ⅳ的线性公式描述=“在线式 “end =”lead“?> H 2 N-OR 3”在线公式描述=“在线公式”end =“tail” 其中R 3'是氢或基团R 3',得到式V的双肟,C)用烷基化剂烷基化V或用酰化酰化V 试剂得到式VI化合物和D)随后的肟基 VI与羟胺的离子,得到式I的化合物。

    Continuous preparation of dimethylvinylcarbinol by isomerizing prenol
    14.
    发明授权
    Continuous preparation of dimethylvinylcarbinol by isomerizing prenol 失效
    通过异构化prenol连续制备二甲基乙烯基甲醇

    公开(公告)号:US06180839B2

    公开(公告)日:2001-01-30

    申请号:US09265923

    申请日:1999-03-10

    CPC classification number: C07C29/56 C07C33/03

    Abstract: A process is described for the continuous preparation of dimethylvinylcarbinol (DMVC) by continuously reacting prenol with the aqueous solution of a protic acid in the still or in the lower part of a rectification column while distilling off the DMVC formed in the form of an azeotropic mixture with water, which comprises a) during the reaction ensuring that as far as possible no liquid two-phase mixture forms in the reaction mixture, b) distilling off the DMVC which forms at a reflux ratio of at least 2, as a result of which there is virtually no more prenol present in the distillate from the column, and c) setting the reaction volume and/or the amount of prenol added per hour and/or the concentration of protons in the reaction mixture in such a manner that the quotient, defined as residence time concentration coefficient, of the reaction volume and the volume of prenol added per hour multiplied by the concentration of protons in the reaction mixture has a value between 0.001 h·mol/l and 1 h·mol/l. In this connection, the formation of a liquid two-phase mixture in the reaction mixture is prevented, in addition to avoiding too large a prenol excess, by continuously taking from the reaction mixture a partial stream, passing it over a phase separation vessel, completely or at least largely removing there the small quantities, formed in the course of the reaction, of organic by-products which are insoluble or only partially soluble in water, and returning the aqueous phase to the reaction volume.

    Abstract translation: 描述了通过在精馏塔的静止或下部连续地反应预先醇与质子酸的水溶液连续反应制备二甲基乙烯基甲醇(DMVC)的方法,同时蒸馏出以共沸混合物形式形成的DMVC 在反应过程中包含a)的水,确保尽可能在反应混合物中形成液体两相混合物,b)蒸发形成回流比至少为2的DMVC,结果是在那里 在柱的馏出物中基本上没有更多的prenol存在,并且c)使反应体积和/或每小时加入的prenol的量和/或反应混合物中的质子浓度设定为使得定义为 停留时间浓度系数,反应体积和每小时加入的prenol体积乘以反应混合物中质子浓度的值为0.001 h.mol / l和 1 h.mol / l。在这方面,防止反应混合物中的液体两相混合物的形成,除了避免过多的过量的过量以外,通过连续取出反应混合物的一部分流,将其通过 在相分离容器中,完全或至少大部分在反应过程中形成的少量去除不溶或仅部分溶于水的有机副产物,并将水相返回到反应体积中。

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