5-氨基噻吩四乙酯的相转移催化合成  

Synthesis of Tetraethyl Ester of 5-Aminothiophene by Phase Transfer Catalysis

作　　者：胡凯 丁翔宇[2] 贾湘曼[2] 蒋晔[2] 刘丰华[2] 

机构地区：[1]河北省邢台市妇幼保健院,河北邢台054000 [2]河北医科大学药学院,石家庄050017

出　　处：《中国现代应用药学》2008年第4期306-307,共2页Chinese Journal of Modern Applied Pharmacy

摘　　要：目的研究了5-氨基噻吩四乙酯的相转移催化合成,并考查最佳催化条件。方法以氧代戊二酸二乙酯为原料,环合生成5-氨基噻吩,再以冠醚为相转移催化剂,溴乙酸乙酯为烷基化试剂,碳酸钾为固体碱,在丙酮中进行烷基化催化反应。结果该催化反应的最佳条件:以冠醚为催化剂,烷基化试剂与固体碱对反应物的摩尔比分别为2.2与2.5,反应温度为60℃(水浴温度),反应时间为6 h。结论此催化反应不良反应少、收率好、纯度高。OBJECTIVE Synthesis of tetraethyl ester of 5-aminothiophene by phase transfer catalysis was studied, and the best catalysis condition was also examinated. METHODS First,5-aminothiophene was synthesized from diethyl acetone-1,3-dicarboxylate by cyclization. Then in acetone, tetraethyl ester of 5-aminothiophene was synthesized from 5-aminothiophene by phase transfer catalysis with ethyl bromoacetate in presence of crown ether using potassium carbonate as solid base. RESULTS The best condition of catalysis was that using crown ether as phase transfer catalyzer, the molar ratio of alkylating reagent, alkali and reagent was 2. 2 and 2.5 respectively, the reaction temperature was 60 ℃ and the time of the reaction was 6 h. CONCLUSION There were many advantages with little side reaction, great yield, and high pure. It was the key preparation for getting high pure strontium ranelate.

关 键 词：相转移催化 烷基化 冠醚 5-氨基噻吩 5-氨基噻吩四乙酯 

分 类 号：R916.41[医药卫生—药学] TQ460.32[化学工程—制药化工]