H_3PW_6Mo_6O_(40)/SiO_2催化合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮

Synthesis of 4-phenyl-6-methyl-5-ethoxycarbonyl-3, 4-dihydropyrimidin-2(H)-one with H_3PW_6Mo_6O_(40)/SiO_2

采用溶胶-凝胶法制备H3PW6Mo6O40/SiO2催化剂,以苯甲醛,乙酰乙酸乙酯和尿素为原料,无水乙醇为溶剂催化合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮,研究结果表明:反应物的摩尔比、反应温度、催化剂用量和反应时间是影响4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮合成收率的重要因素.当n(苯甲醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1.0∶1.2∶1.5,反应温度为90℃,催化剂的用量占反应物料总质量的1.5%,反应时间为75min时,产品收率可达70.3%.通过熔点、IR、1 H NMR和MS对合成目标化合物进行了表征确认.

4-Phenyl-6-methyl-5-ethoxycarbonyl-3,4-dihydropyrimidin-2-（H）-one was synthesized with a new catalyst, H3PW6Mo6O40/SiO2 prepared by a sol-gel technique. The influence factors of reaction conditions on the yield of the product were discussed and the best reaction conditions were shown as follows： under the condition of fixed benzaldehyde consumption was 0. 04 mol and anhydrous ethanol is 15 mL, n （benzaldehyde） ： n （ethylacetoacetate） ： n（urea）=1. 0 ： 1. 2 ： 1. 5, reaction temperature was 90 ℃, mass fraction of catalyst to reactants was 1. 5%, and reaction time was 75 min. The yield of the product could reach 70. 3%. The 3,4- dihydropyrimidin-2（H）-one were characterized by melting point measurements, IR, 1H NMR and MS spectroscopy.