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噻托溴铵的合成
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.
作者姓名:靳凤民  张静
作者单位:1. 天津大学化工学院, 天津 300072; 2. 天津大学仁爱学院, 天津 301636
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):n2(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。

关 键 词:噻托溴铵    溴甲烷    合成

Synthsis of Tiotropium Bromide
Affiliation:1. School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China; 2. Renai College of Tianjin University, Tianjin 301636, China
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    
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