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9h。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1 H NMR进行了表征。
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 reac- tion temperature, reaction time, types of catalyst and solvent on reaction results were examined. The obtained optimum conditions were using copper powder as catalyst, DM- SO 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.
出处
《青岛科技大学学报(自然科学版)》
CAS
北大核心
2012年第5期449-453,共5页
Journal of Qingdao University of Science and Technology:Natural Science Edition
关键词
3
4-乙烯二氧噻吩
脱羧反应
正交试验
3,4-ethylene dioxy thiophene
decarboxylation
orthogonal test
作者简介
冯柏成(1965-),男,副教授.