2-氨基-4-甲基-5-甲酰乙氧基噻唑氢溴酸盐的合成

Synthesis of Ethyl 2-Amino-4-Methylthiazole-5-Carboxylate

乙酰乙酸乙酯和液溴的四氯化碳溶液回流,溴代反应2 h后,减压蒸馏得到溴代乙酰乙酸乙酯,产率80.1%.将硫脲溶于乙醇中,加入溴代乙酰乙酸乙酯进行环合反应12 h,通过减压蒸馏、重结晶进行分离提纯得到2_氨基_4_甲基_5_甲酰乙氧基噻唑氢溴酸盐.用元素分析、红外光谱、核磁共振氢谱、质谱等方法对合成产物进行了表征,证明所得到的产物具有预期的结构.

Acetacetic este was refluxed with a solution of Br2 in CCl4 for 2 h and then vacuum distillated to give 4-bromo-acetacetie ester in 80.1% yield. A solution of thiourea in alcohol was put into 4-bromo acetacetie ester and then refluxed for 12 h, vacuum distillated to remove alcohol, reerystallized to give ethyl 2-amino-4-methylthiazole-5-carboxylate in 62% yield. It was identified by elemental analysis, FT-IR, ^1H NMR and MS.