富马酸依美斯汀原料药合成工艺的改进及其结构表征  

Improved Synthetic Method and Characterization of Emedastine Difumarate

作　　者：李艳芹[1] 于凤丽[2] 庄胜利 

机构地区：[1]杭州民生药业有限公司,杭州310011 [2]青岛科技大学化学与分子工程学院,青岛266042

出　　处：《应用化学》2013年第11期1285-1288,共4页Chinese Journal of Applied Chemistry

摘　　要：以邻苯二胺为起始原料,经5步反应合成了富马酸依美斯汀(1)。采用加入相转移催化剂的方法,改进了2个关键中间体2-氯-1-(2-乙氧基乙基)苯并咪唑(4)和依美斯汀(5)的合成工艺。反应无需控制水分,中间体4和5的收率分别提高至67.9%和74.9%。产物的结构经IR、1H NMR、13C NMR、质谱、元素分析、差热分析及X射线粉末衍射证实。Emedastine difumarate （1） was prepared via improved synthetic processes. After adding phase transfer catalyst, the synthesis of the two key intermediates such as 2-chloro-l-（2-ethoxyethyl） benzimidazole （4） and emedastine（5 ） for the reactions could be optimized. No water was needed for the reactions and the yields were significantly enhanced. Typically, the yields of compounds 4 and 5 are up to 67.9% and 74.9%, respectively. The structure of the prepared product was confirmed by IR, ^1H NMR, 13C NMR, MS, elemental analysis, differential thermal analysis, and X-ray powder diffraction.

关 键 词：富马酸依美斯汀 合成 表征 相转移催化剂 

分 类 号：O621.3[理学—有机化学]