摘要
以芳香醛、乙酰乙酸乙酯及脲为原料,I2负载蒙脱土为催化剂,对超声条件下Biginelli反应进行研究。用单因素法考察溶剂及催化剂对产率的影响,通过正交试验优化温度、超声时间及原料摩尔比。优化反应条件为:反应温度80℃,超声时间5min,芳香醛、乙酰乙酸乙酯和脲的摩尔比为1∶1∶1,催化剂用量为10(mol)%,产率最高可达86.9%。合成的7种3,4-二氢嘧啶-2(1H)-酮衍生物的结构通过红外光谱、核磁共振氢谱和熔点进行表征。
An ultrasound-assisted Biginelli reaction catalysized by I2 loaded montmorillonite was developed using ethylacetoacetate,aromatic aldehyde and urea as starting materials. Influences of solvents,catalysts on the yield were investigated using single factor methods,and the temperature,ultrasonic time,equivalent ratio of starting materials were screened using orthogonal tests. Under the optimized conditoin,the yields of 3,4-dihydropyrimidin-2（ 1H） one derivatives were up to 86. 9%. The products were characterized by^1 H NMR,IR and m. p.
出处
《化学通报》
CAS
CSCD
北大核心
2016年第9期834-838,共5页
Chemistry
基金
国家自然科学基金项目(21362006)
贵州省科学技术基金项目(黔科合J字[2014]2129)资助
