Process for the separation of isomeric cyclopropane-carboxylic acids
    3.
    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。

    Process for preparing 2-guanidinomethyl-perhydroazocine-sulfate
    4.
    发明授权
    Process for preparing 2-guanidinomethyl-perhydroazocine-sulfate 失效
    2-胍基甲基 - 全氢化ine硫酸盐的制备方法

    公开(公告)号:US4065450A

    公开(公告)日:1977-12-27

    申请号:US661613

    申请日:1976-02-26

    IPC分类号: C07D225/02 C07D223/04

    CPC分类号: C07D225/02

    摘要: The invention relates to a novel process for preparing 2-guanidinomethyl-perhydroazocine-sulfate of formula I ##STR1## comprising the steps of catalytically reducing the 2-nitromethylene-perhydroazocine of formula IV ##STR2## in solution in acetone at a temperature of 20.degree. to 50.degree. C, treating the separated reaction product with an aqueous mineral acid and then reacting it with S-methyl-isothiocarbamid-sulfate.The process gives the desired end-product of formula I also on industrial scales.

    摘要翻译: 本发明涉及一种制备式I的2-胍基甲基 - 全氢化ine硫酸盐的新方法,其包括以下步骤:在丙酮溶液中,在丙酮溶液中催化还原2-硝基亚甲基 - 全氢az嗪, 20℃至50℃,用无机酸水溶液处理分离的反应产物,然后与S-甲基 - 异硫代氨基甲酰硫酸盐反应。