噻托溴铵的合成

摘要

以2(2-噻吩基)乙醇酸东莨菪酯(TB-1)和溴甲烷为原料合成了噻托溴铵。探索了反应时间、反应温度、反应配比等反应条件对于反应收率的影响。结果表明最适宜合成工艺条件为:反应温度21~25 ℃,反应时间5 h,物料配比n(二乙基甲氧基硼烷):n[2(2-噻吩基)乙醇酸东莨菪酯]为3:1。在最适宜工艺条件下制得产品为白色固体,熔点为218.0~219.3 ℃,产率在95%以上。并通过质谱和核磁共振对其进行了结构表征。

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	靳凤民
	张静

关键词：噻托溴铵；溴甲烷；合成

Abstract：

Tiotropium bromide was prepared from TB-1 and bromomethane. The effects of reaction time, temperature and molar ratio of the material on the reaction were studied. The experimental result showed that the optimum condition were: reaction time was 5 h, reaction temperature was 21—25 ℃, molar ratio of bromomethane to TB-1 was 3:1. The product was white solid with melting point of 218.0—219.3 ℃, the yield of product was up to 95%. MS and NMR were used to characterize the structure of product.

Keywords： tiotropium bromide； bromomethane； synthesis

Received 2014-11-30;

Corresponding Authors: 张静, E-mail: helenzhang2009@126.com。 Email: helenzhang2009@126.com

About author: 靳凤民(1978-),男,工程师,主要研究方向为精细化学品的合成,纳米材料分析及表征。

引用本文:

靳凤民, 张静.噻托溴铵的合成[J]. 化学工业与工程, 2016,33(1): 57-60

Jin Fengmin, Zhang Jing.Synthsis of Tiotropium Bromide[J]. Chemcial Industry and Engineering, 2016,33(1): 57-60

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