硫酸铜微波催化合成己二酸二乙酯工艺的优化

Optimization of Copper Sulfate Catalytic Synthesis of Diethyl Adipate by Microwave Technology

己二酸二乙酯是有机合成中重要的溶剂和中间体,其合成是以己二酸和乙醇为原料,硫酸铜催化下,78℃左右在微波萃取仪中加入0.012 mol己二酸,11.2 m L乙醇,再加入10 m L苯,通过改变不同的催化剂用量、反应时间、己二酸与乙醇的配比、微波功率等条件,探究出一条高产率的合成路线。即:最佳实验条件为:酸∶醇=1∶8、硫酸铜1.0 g、反应时间12 min、微波功率700 W。通过IR表征初步证明产物为己二酸二乙酯。

Diethyl adipate is an important solvent and intermediates in organic synthesis. Its synthesis used adipic acid and ethanol as raw material,copper sulfate as catalyst in the condition of 78 ℃,the microwave radiometer with0. 012 mol adipic acid and 11. 2 m L ethanol,and then joined the 10 m L by changing the conditions of benzene,amount of catalyst,reaction time,raw material ratio of adipic acid with ethanol,different microwave power,to explore the synthesis route with high yield. The best experiment conditions were as follows： acid ∶ alcohol = 1∶8,copper sulfate was 1. 0 g,reaction time was 12 min,microwave power was 700 W. The IR characterization showed that product of the synthesis was diethyl adipate.