3-(2-噻吩)丙烯酸的合成工艺优化

Synthesis Process Optimization of 3-(2-Thienyl) acrylic Acid

以噻吩-2-甲醛为原料,经磷酰基乙酸三乙酯活化酯化、水解两步合成了3-(2-噻吩)丙烯酸,优化了合成工艺,产物总收率达95.5%。研究了活化酯化反应中噻吩-2-甲醛与膦酰基乙酸三乙酯的物质的量比,当两者比例为1∶1.05时,噻吩-2-甲醛的转化率最高,大于99.0%;研究了水解过程中氢氧化钾用量、氢氧化钾浓度、反应温度和反应时间的影响,得出最佳的水解条件为:氢氧化钾与3-(2-噻吩)丙烯酸乙酯物质的量比为4∶1、氢氧化钾浓度为4mol/L、反应温度为40℃、反应时间为4小时。

Using2-thenaldehyde as starting material,3-(2-Thienyl)acrylic acid with total yield of95.5%was synthesized via triethyl phosphonoaeetate activated esterification and hydrolysis.The synthesis process was optimized.In the activated esterification reaction,mole ratio of2-thenaldehyde and triethyl phosphonoaeetate was studied.When the ratio was1:1.05,the conversion of2-thenaldehyde was over99.0%.In the hydrolysis reaction,KOH dosage,mole ratio of KOH and ethyl3-(2-thienyl)acrylate,potassium hydroxide concentration,temperature and reaction time were studied.The result showed that the optimum reaction condition was as follows:mole ratio of KOH and ethyl3-(2-thienyl)acrylate4:1,potassium hydroxide concentration4mol/L,40℃,4hours.