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2012050449冯柏成， 张庆云， 李同全
（青岛科技大学 化工学院， 山东 青岛 266042）
摘要： 以2,5-二羧酸-3,4-乙烯二氧噻吩为原料，经过催化脱羧反应合成聚合物单体3,4-乙烯二氧噻吩。通过对催化剂、溶剂、反应温度及反应时间4个因素的改变，对其合成工艺进行了优化。实验结果表明，脱羧反应的最佳工艺条件为：铜粉为催化剂，DMSO为溶剂，反应温度160 ℃，反应时间9 h。在此条件下，产品的收率为68%，纯度为99.5 %。目标化合物的结构通过GC-MS和1H NMR进行了表征。
关键词: 3,4-乙烯二氧噻吩； 脱羧反应； 正交试验
中图分类号： TQ 612.6文献标志码： A
收稿日期：2012-01-05
作者简介： 冯柏成（1965—），男，副教授.
Preparation of 3,4-Ethylene Ddioxy Thiophene by Catalytic Decarboxylation
FENG Bai-cheng, ZHANG Qing-yun, LI Tong-quan
（College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China）
Abstract: 3,4-Ethylene dioxy thiophene was prepared by catalytic decarboxylation using 2,5-dicarboxylic acid-3,4-ethylene dioxy thiophene as raw material. The effects of reaction temperature, reaction time, types of catalyst and solvent on reaction results were examined. The obtained optimum conditions were using copper powder as catalyst, DMSO as solvent, reaction temperature 160 ℃, reaction time 9 h. Under above conditions, the yield and purity of product were 68% and 99.5% respectively. The structure of the product was characterized by GC-MS and 1H NMR.
Key words: 3,4-ethylene dioxy thiophene; decarboxylation; orthogonal test
