铜/中孔二氧化硅催化合成2，2-二甲基环丙烷甲酸乙酯

SYNTHESIS OF ETHYL-2,2-DIMETHYLCYCLOPROPANE-CARBOXYLATE ON COPPER/MESOPOROUS SILICA CATALYST

以甘氨酸、无水乙醇和异丁烯等为原料,经酯化、重氮化、环丙烷化三步反应合成2,2-二甲基环丙烷甲酸乙酯。采用中孔二氧化硅(CFG)负载铜离子为催化剂,探讨了环丙烷化的反应温度、反应时间、负载铜与非负载铜及催化剂用量对收率的影响。结果表明,当反应温度50℃,反应时间130min时,铜氨络离子与CFG交换后经100℃处理过的Cu/CFG其催化活性最高,收率38.9%;而以铜盐为催化剂时,收率10.4%。催化剂负载后可降低铜盐用量,而且Cu/CFG易于分离,可再生使用。

Using aminoacetic acid, absolute alcohol and isobutene as raw material, ethyl-2,2-dimethylcyclopropanecarboxylate was synthesized via esterification, diazo-reaction and cycloproanation. The copper catalyst was modified for pivotal cyclopropanantion reaction and copper/mesoporous silica（Cu/ CFG） catalyst was prepared by ion exchange process. The influence of factors such as temperature, reaction time, loaded or unloaded Cu catalyst and the dosage on the yield of products were investigated. The results indicated that Cu/CFG handled at 100 ℃ after the ion exchange displayed higher conversion at 50 ℃, reaction time of 130 min and the yield is 38.9%. However, cupric salt as catalyst, the highest yield is 10.4%. Furthermore, Cu/CFG is easily separated, recycled and reducing the consumption of cupric salt.