药物中间体二苯甲基-3-氰基胍的制备  

Preparation of Drug Intermediate 1,1-Diphenylmethyl-3-cyanoguanidine

作　　者：李卓雅 殷小龙 朱展 黄小杉 刘忠湃 张科良[1] LI Zhuoya;YIN Xiaolong;ZHU Zhan;HUANG Xiaoshan;LIU Zhongpai;ZHANG Keliang(College of Chemisitry&Chemical Engineering,Xi’an Shiyou University,Xi’an 710065,China)

机构地区：[1]西安石油大学化学化工学院,陕西西安710065

出　　处：《化工技术与开发》2023年第5期16-18,28,共4页Technology & Development of Chemical Industry

基　　金：陕西省大学生科技创新项目(S202110705124)。

摘　　要：本文以二苯基甲胺盐酸盐和二氰胺钠为原料,在正丁醇溶剂中合成了药物中间体二苯甲基-3-氰基胍。采用单因素研究法,探究了反应物配比、反应温度、反应时间、溶剂用量对产品收率的影响。最佳制备工艺条件为:反应时间为6h,n(二苯甲胺盐酸盐)∶n(二氰胺钠)=1∶1.15,反应温度为120℃,溶剂用量为50m L,此条件下的收率为94%。在此基础上进行了底物拓展研究。对粗产品进行了分离精制,对纯化的产品进行了IR分析、^(1)H NMR及^(13)C NMR结构表征。结果表明,制备的产物与预期的结构相符。The pharmaceutical intermediate 1,1-diphenylmethyl-3-cyanoguanidine was prepared through reaction of diphenylmethylamine hydrochloride and sodium dicyandiamide using n-butanol as solvent.Single factor study was used to investigate the effects of reactant ratio,reaction temperature,reaction time,solvent dosage on the reaction yields.The optimum preparation conditions were as followed:reaction time 6h,reaction temperature 120℃,the solvent dosage 50ml,n(diphenylamine hydrochloride):n(sodium dicyandiamide)=1.1.15.Under these conditions,the yield was 94%.On this basis,the study of substrate extension were carried out.The crude product were separated and refined.The purified product were characterized by IR,^(1)H NMR and ^(13)C NMR.The results showed that the prepared product were in accordance with the expected structure.

关 键 词：二苯甲胺盐酸盐 二氰基胺钠 合成 柱分离 结构表征 

分 类 号：TQ226.3[化学工程—有机化工] R914.5[医药卫生—药物化学]