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    • 93. 发明授权
    • Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane
    • 制备1,6-二(N 3 - 氰基-N 1胍基)己烷的方法
    • US5041655A
    • 1991-08-20
    • US241116
    • 1988-09-06
    • Klaus HuthmacherAxel KleemannHorst BethgeRolf Braun
    • Klaus HuthmacherAxel KleemannHorst BethgeRolf Braun
    • C07C67/00C07C239/00C07C277/08C07C279/28
    • C07C279/28
    • An improved method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane from alkali dicyanamide and a hexamethylene diammonium salt in alcoholic solution or suspension. The reaction is carried out in the presence of a limited amount of water and of a catalytic amount of a base, preferably a tertiary amine. The pH of the reaction mixture at the start of the reaction is 8 to 10. After the reaction is over, the reaction mixture is compounded with water at a temperature above 80.degree. C. and the coarse product which crystallizes out is separated from the liquid phase.Preferably, sodium dicyanamide and hexamethylene diamine dihydrochloride, preferably formed in situ from aqueous 1,6-diaminohexane and aqueous hydrochloric acid, are reacted at pH 9-9.5 in n-butanol in the presence of 0.1 to 20% by wt. water in relation to the solvent including water.1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane is obtained in a high yield (85-86%) and with great purity (95-97%) and with a considerably improved space-time yield.
    • 一种在醇溶液或悬浮液中由碱二氰胺和六亚甲基二铵盐制备1,6-二(N 3 - 氰基-N 1胍基)己烷的改进方法。 反应在有限量的水和催化量的碱,优选叔胺的存在下进行。 反应开始时反应混合物的pH值为8〜10。反应结束后,将反应混合物在高于80℃的温度下与水混合,将结晶出来的粗产物与液体分离 相。 优选地,优选在1,6-二氨基己烷水溶液和盐酸水溶液中原位形成的二氰胺钠和六亚甲基二胺盐酸盐在pH为9-9.5的正丁醇中,在0.1-20重量%的存在下反应。 相对于包括水在内的溶剂的水。 以高产率(85-86%)和高纯度(95-97%)获得1,6-二(N 3 - 氰基-N 1胍基)己烷,并具有显着提高的时空产率。