超声波下4-甲基-6-苯基-5-乙氧羰基-3,4-二氢嘧啶-2-硫酮的合成研究

Study on Synthesis of 4-methyl-6-phenyl-5-ethoxycarbonyl-3,4-dihypyrimidine-2-sulfur Ketone under Ultrasonic Irradiation

超声波辐射下利用Biginelli缩合反应,以苯甲醛、乙酰乙酸乙酯和硫脲为原料,对甲苯磺酸为催化剂合成4-甲基-6-苯基-5-乙氧羰基-3,4-二氢嘧啶-2-硫酮.探究反应物的配比、溶剂种类、反应温度、催化剂用量等因素对产率的影响,得到较佳合成条件:无溶剂,对甲苯磺酸0.50g,温度65℃,原料配比n苯甲醛:n乙酰乙酸乙酯:n硫脲=1.0:1.0:1.0,产率37.7%,并对产物进行了初步表征.

Under ultrasonic irradiation,4-methyl-6-phenyl-5-ethoxycarbonyl-3,4-dihypyrimidine-in-2-sulfur ketone was synthesized by Biginelli condensation reaction using benzaldehyde,ethyl acetoacetate and thiourea as raw materials,p-toluenesulfonic acid as catalyst.The optimum reaction conditions of ultrasonic radiation were obtained by exploring the influence of the ratio of raw materials,the kind of solvent,reaction temperature and the amount of catalyst of the reaction on the yield.The result is p-toluenesulfonic acid as a c-atalyst and an amount of 0.5 g,the temperature(65℃),no solvent,ratio of raw materials(1.0︰1.0︰1.0),the yield(37.7%).The production was preliminary characterized.