一锅法合成2-(5-氨基-1,3,4-噻二唑)基丙酸乙酯

One-Pot Synthesis of Ethyl-(5-amino-1,3,4-thiadiazol-2-yl) Propionate

以丁二酸酐和氨基硫脲为原料,采用"一锅法"经脱水环合合成了重要医药中间体2-(5-氨基-1,3,4-噻二唑)基丙酸乙酯,其结构经~1H NMR,IR和MS确证。并对反应条件进行了优化,最佳反应条件为∶n(氨基硫脲)∶n(丁二酸酐)∶n(浓硫酸)=1∶2∶3,于80℃反应6 h,收率70%。

The important pharmaceutical intermediate,ethyl-(5-amino-1,3,4-thiadiazol-2-yl)propionate with yield of 70%,was synthesized by one-pot method,using succinic anhydride and thiosemicarbazide as starting materials.The structure was confirmed by 1 H NMR,IR and MS.The reaction conditions were optimized by orthogonal test.The results showed that the optimal reaction conditions were as follows n(thiosemicarbazide)∶n(succinic anhydride)∶n(concentrated sulfuric acid)=1∶2∶3,reaction at 80℃for 6 h.