摘要
以取代水杨醛和氰乙酸酯为原料，以水或体积分数约50％乙醇为溶剂，以K2CO3为催化剂合成了6个2-氨基-4H-色烯衍生物。以水杨醛与氰乙酸乙酯的反应为模板反应，通过单因素实验优化了反应条件。结果表明，水杨醛10mmol，水杨醛与氰乙酸酯的摩尔比为1：2．5，K2CO3用量1mmol，20mL水作溶剂，40℃恒温水浴中搅拌反应40min，获得产率高达94．2％的目标产物，催化剂重复使用5次，其催化活性下降不明显。当以氰乙酸甲酯代替氰乙酸乙酯反应，得到相应目标物的产率为90．1％；当以固态5-溴（或氯）-水杨醛代替水杨醛与氰乙酸酯在20mL约50％乙醇作溶剂反应时，获得相应目标物的产率为78．9％～86．6％。
Six 2-amino-4H-chromene derivatives were synthesized from the substituted salicylaldehyde and cyanoacetate in the presence of water or 50% ethanol solution catalyzed by KECO3. With salicylaldehyde and ethyl cyanoacetate as template reaction, the reaction conditions were optimized by single factor experiments. The results show that the target product was obtained in 94. 2% yield based on 10 mmol of salicylaldehyde, molar ratio of salicylaldehyde to ethyl cyanoaeetate 1：2.5, dosage of K2C03 1 mmol,20 mL water as solvent and reaction time 40 min in water bath of 40 ~C constant temperature. The catalyst solution can be reused for 5 cycles without significant loss of activity. When methyl cyanoacetate displaced ethyl cyanoacetate, the corresponding target product was synthesized with a yield of 90. 1%. When solid 5-bromo（ or chloro） -salicylaldehyde displaced salicylaldehyde at 20 mL 50% ethanol solution as solvent, the corresponding target products were synthesized with a yield ranging between 78.9% ～86.6%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2014年第12期1522-1525,1530,共5页
Fine Chemicals
基金
嘉应学院自然科研基金项目(2014KJY04)~~
