摘要
以甘氨酸乙酯盐酸盐为原料和丙烯腈进行加成反应,氨基保护,然后在乙醇钠存在下发生Dieckmann环化反应.通过对各步反应进行研究、优化,得到最佳反应条件.加成反应:丙烯腈与甘氨酸乙酯盐酸盐的投料摩尔比为2.5∶1,反应温度55℃,时间6 h.收率为66.0%.合环反应:选择乙醇钠为合环剂.对中间体进行了核磁共振氢谱、元素分析等表征,结果表明,各产品的化学结构与目标产物相符.
The addition reaction of glycine ethyl ester with acrylonitrile and the amino group protecting reaction were carried out, then the Dieckmann cyclization occurred with the action of sodium alkoxides. The results of the studies showed that the optimal addition reaction condition was : acrylonitrile : glycine ethyl ester (mol) is 2.5 : 1, reaction temperature is 55℃, reaction time is 6h. The recovery was 66.0% under this condition, the optimal condition of Dieckmann cyclization reaction was to select sodium alkoxides to promote the cyclization. The intermediate was analyzed with nuclear magnetic resonance, the result showed that the chemical structure of the products coincide with the aim product.
出处
《河南工业大学学报(自然科学版)》
CAS
北大核心
2005年第4期28-31,共4页
Journal of Henan University of Technology:Natural Science Edition