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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。
Aromatic aldehydes, ethyl acetoacetate and urea as raw materials, I2-loaded montmorillonite as a catalyst, the Biginelli reaction under ultrasound conditions were studied. The effects of solvent and catalyst on the yield were investigated by single factor method. The orthogonal test was used to optimize the temperature, ultrasonic time and molar ratio of raw materials. The optimized reaction conditions were as follows: the reaction temperature was 80 ℃, the ultrasonic time was 5 min, the molar ratio of aromatic aldehyde, ethyl acetoacetate and urea was 1: 1:1, the amount of catalyst was 10 (mol)% and the yield was up to 86.9%. The structures of 7 synthesized 3,4-dihydropyrimidin-2 (1H) -one derivatives were characterized by IR, 1H NMR and melting point.