应用化学

• 研究论文 • 上一篇    下一篇

富马酸依美斯汀原料药合成工艺的改进及其结构表征

李艳芹1*,于凤丽2,庄胜利1   

  1. (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)
  • 收稿日期:2012-12-24 修回日期:2013-03-11 出版日期:2013-11-10 发布日期:2013-11-10
  • 通讯作者: 李艳芹,高级工程师; Tel:0571-89973633-248; Fax:0571-88840407 ; E-mail:lyqin@mspharmcom; 研究方向:药物化学研究及新药的开发

Improved Synthetic Method and Characterization of Emedastine Difumarate

LI Yanqin1*, YU Fengli2, ZHUANG Shengli1   

  1. (1.Hangzhou Minsheng Pharmaceutical Group Co.,Ltd.,Hangzhou 310011,China;
    2.College of Chemistry and Molecular Engineering,Qingdao University of Science and Technology,Qingdao 266042,China)
  • Received:2012-12-24 Revised:2013-03-11 Published:2013-11-10 Online:2013-11-10

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。

关键词: 富马酸依美斯汀, 合成, 表征, 相转移催化剂

Abstract: 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-1-(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.

Key words: Emedastine difumarate, synthesis, characterization, phase transfer catalysts

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