| 富马酸依美斯汀原料药合成工艺的改进及其结构表征 |
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| 引用本文： | 李艳芹,于凤丽,庄胜利.富马酸依美斯汀原料药合成工艺的改进及其结构表征[J].应用化学,2013,30(11):1285-1288. |
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| 作者姓名： | 李艳芹 于凤丽 庄胜利 |
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| 作者单位： | (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) |
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| 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。
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| 关 键 词： | 富马酸依美斯汀 合成 表征 相转移催化剂 |
| 收稿时间： | 2012-12-24 |
| 修稿时间： | 2013-03-11 |
Improved Synthetic Method and Characterization of Emedastine Difumarate |
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| LI Yanqin,YU Fengli,ZHUANG Shengli.Improved Synthetic Method and Characterization of Emedastine Difumarate[J].Chinese Journal of Applied Chemistry,2013,30(11):1285-1288. |
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| Authors: | LI Yanqin YU Fengli ZHUANG Shengli |
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| Institution: | (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) |
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| 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. |
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| Keywords: | Emedastine difumarate synthesis characterization phase transfer catalysts |
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