米拉贝隆中间体2-氨基噻唑-4-乙酸的合成  

Synthesis of The Intermediate for Mirabegron Aminothiazole-4-2-ethyl Acetic Acid

作　　者：黄婷[1] 徐啸波 张纯宝 张华华[1] 

机构地区：[1]大连理工大学(盘锦)石油与化学工程学院,辽宁盘锦124221 [2]衢州爱美康生物科技有限公司,浙江衢州324000

出　　处：《合成化学》2017年第5期437-439,共3页Chinese Journal of Synthetic Chemistry

基　　金：辽宁省科技攻关项目(2015220034);大连理工大学大学生创新实验项目(U20161193)

摘　　要：以氰胺、硫和氯乙酰乙酸乙酯为原料,一水合对甲苯磺酸(TsOH·H_2O)为催化剂,经成环反应制得2-氨基噻唑-4-乙酸乙酯(2);2经水解反应合成了米拉贝隆中间体2-氨基噻唑-4-乙酸,其结构经~1H NMR,^(13)C NMR,IR和元素分析确证。在最佳反应条件[10.25 mol,TsOH·H_2O 0.01 mol,反应温度为80℃,重结晶溶剂(乙醇/水=1/1,V/V)]下,2收率88.2%。Amino thiazole-4-2-ethyl acetate（2） was obtained by cyclization reaction, using cyanam- ide, elemental sulfur and chlorine ethyl acetoacetate as the starting materials, and TsOH H2O as the catalyst. The intermediate for Mirabegron, aminothiazole-4-2-acetic acid, was synthesized by hydroly- sis reaction of 2. The structure was confirmed by 1H NMR, 13C NMR, IR and elemental analysis. The yield of 2 was 88.2% under the optimum reaction conditions[ 1 0.25 mol, TsOH H2O 0.01 tool, reaction at 80℃, the recrystallization solvent was （ EtOH/H2O = 1/1, V/V） ].

关 键 词：氯乙酰乙酸乙酯 2-氨基噻唑-4-乙酸 米拉贝隆 中间体合成 

分 类 号：O626.25[理学—有机化学] R914.5[理学—化学]