Preparation of cyclopropanecarboxylic acid esters
    1.
    发明授权
    Preparation of cyclopropanecarboxylic acid esters 失效
    制备环丙烷羧酸酯

    公开(公告)号:US4299972A

    公开(公告)日:1981-11-10

    申请号:US164902

    申请日:1980-07-01

    CPC分类号: C07C69/743

    摘要: A process is disclosed for the preparation of an optically active or racemic cyclopropanecarboxylic acid of the formula (I) ##STR1## wherein R.sup.1 and R.sup.2 are the same or different and each is lower alkyl or halogen;R is a member of a group which contains various cyclic structures as set forth in the specification,the .about. valency bond represents .alpha.- and/or .beta.-configuration;the -- valency bond represents .beta.-configuration,which comprises reacting an optically active or racemic cyclopropanecarboxylic acid of the formula (VII) ##STR2## with a dimethyl-methylidene-ammonium salt of the formula (VIII) ##STR3## wherein X is halogen or lower alkoxy andY.sup.- is a halide or lower alkylsulfate ion in an anhydrous, inert organic solvent, and sebsequently reacting a dimethyl-acloxy-methylidene-ammonium salt thus obtained with an optically active, inactive or racemic alcohol of the formulaR--OHwithout isolation, in the presence of an organic base.

    摘要翻译: 公开了制备式(I)的光学活性或外消旋环丙烷羧酸的方法,其中R 1和R 2相同或不同,各自为低级烷基或卤素; R是包含说明书中所列的各种环状结构的基团的成员,差异化合价键代表α-和/或β-构型; 价键表示β构型,其包括使式(VII)的光学活性或外消旋环丙烷羧酸与式(VIII)的二甲基亚甲基铵盐反应(VIII) )其中X是卤素或低级烷氧基,Y-是在无水惰性有机溶剂中的卤化物或低级烷基硫酸根离子,然后使由此得到的二甲基 - 酰氧基 - 亚甲基 - 铵盐与光学活性的无活性或外消旋醇反应 式R-OH不分离,在有机碱的存在下。

    Process for the preparation of trichloromethyl carbinols
    5.
    发明授权
    Process for the preparation of trichloromethyl carbinols 失效
    制备三氯甲基甲醇的方法

    公开(公告)号:US4999454A

    公开(公告)日:1991-03-12

    申请号:US784692

    申请日:1985-10-03

    摘要: The invention is directed to a new process for the preparation of carbinols of the general formula I ##STR1## by reaction chloral and olefins of the general formula ##STR2## and by optional acylation of the product comprising dissolving a catalyst of the general formula IIIFe.sub.n (NH.sub.4).sub.x Y.sub.m .multidot.A.sub.p IIIin chloral, then adding the olefin of the general formula II in order to produce a complex of the general formula IV ##STR3## from which a complex of the general formula V ##STR4## is formed, and from the reaction mixture a compound of the general formula I is obtained whereafter(a) the residual complex of the general formula V dissolved in the product is decomposed with an acidic solution and if desired the obtained product is distilled or(b) the product in the reaction mixture is acylated.The compounds prepared according to the invention can be utilized as intermediates when preparing e.g., permethrin and other pyrethroid insecticides.

    摘要翻译: 本发明涉及一种通过反应式I和通式II的烯烃制备通式I的甲醇的新方法,并通过产物的任意酰化,包括将通式 III Fen(NH4)xYmxAp III,然后加入通式II的烯烃以产生通式IV的复合物IV,其中形成通式V的复合物V, 并且从反应混合物中获得通式I的化合物,之后(a)溶解在产物中的通式V的残余络合物用酸性溶液分解,如果需要,所得产物被蒸馏,或(b)产物 在反应混合物中进行酰化。 当制备例如氯菊酯和其他拟除虫菊酯杀虫剂时,根据本发明制备的化合物可以用作中间体。

    Process for the separation of isomeric cyclopropane-carboxylic acids
    10.
    发明授权
    Process for the separation of isomeric cyclopropane-carboxylic acids 失效
    异构环丙烷羧酸分离方法

    公开(公告)号:US4599444A

    公开(公告)日:1986-07-08

    申请号:US581081

    申请日:1984-02-17

    CPC分类号: C07C51/487

    摘要: The invention relates to a new process for separating the four stereoisomers of the cyclopropanecarboxylic acids of the formula ##STR1## wherein R stands for a methyl group or a halogen atom.The process comprisesreacting a salt formed with an alkali hydroxide or an alkali carbonate of dl-cis-trans-2,2-dimethyl-3-(2,2-disubstituted vinyl)-cyclopropanecarboxylic acids containing the isomers in any ratio or the pure dl-cis and dl-trans-2,2-dimethyl-3-(2,2-disubstituted vinyl)-cyclopropanecarboxylic acids prepared therefrom by the means of a selective dissolution with aromatic and aliphatic hydrocarbon solvents (suitably with benzene, extraction petroleum ether, n-hexane) with N-benzyl-2-aminobutanol enantiomers or with the hydrochlorides thereof in an aqueous medium or aqueous acetone medium, obtaining the crystalline diastereomeric salt from the solution by filtration, decomposing said salt by using a mineral acid, then separating the thus obtained optically active cyclopropanecarboxylic acidand obtaining the other isomer or other mixture of isomers from the filtrate of the said diastereomeric salt similarly after acidifying by a mineral acid, if desired, purifying the said optically active 2,2-di-methyl-3-(2,2-disubstituted vinyl)-cyclopropane-carboxylic acid isomers obtained by the above-mentioned procedure by a selective precipitation and recovering the resolving agent.

    摘要翻译: 本发明涉及用于分离式(I)的环丙烷羧酸的四种立体异构体的新方法,其中R代表甲基或卤素原子。 该方法包括使含有任何比例的异构体的dl-顺 - 反-2,2-二甲基-3-(2,2-二取代的乙烯基) - 环丙烷羧酸的碱金属氢氧化物或碱金属碳酸盐形成的盐或纯的 dl-顺式和dl-反式-2,2-二甲基-3-(2,2-二取代的乙烯基) - 环丙烷羧酸,其通过选择性溶解与芳族和脂族烃溶剂(适合于苯,萃取石油醚 正己烷)与N-苄基-2-氨基丁醇对映体或其盐酸盐在水性介质或丙酮水溶液中反应,通过过滤从溶液中获得结晶非对映体盐,通过使用无机酸分解所述盐,然后分离 由此获得的光学活性环丙烷羧酸,并从所述非对映异构体盐的滤液中得到其它异构体或其它异构体混合物,同样地在无机酸酸化后,如果需要, 通过选择性沉淀获得的通过上述方法获得的光学活性的2,2-二甲基-3-(2,2-二取代的乙烯基) - 环丙烷 - 羧酸异构体并回收拆分剂。