H_3PW_(12)O_(40)/SiO_2催化一锅法合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮  

The one-pot synthesis of 4-phenyl-6-methyl-5-ethoxycarbonyl-3,4-dihydropyrimidin-2(H)-one using H_3PW_(12)O_(40)/SiO_2 as catalyst

作　　者：朱雅婷[1] 于颍[1] 龚文朋[1] 徐玉林[1] 杨水金[1] 

机构地区：[1]湖北师范学院化学化工学院,污染物分析与资源化技术湖北省重点实验室,湖北黄石435002

出　　处：《宝鸡文理学院学报（自然科学版）》2014年第3期17-21,共5页Journal of Baoji University of Arts and Sciences(Natural Science Edition)

基　　金：污染物分析与资源化技术湖北省重点实验室开放基金资助项目(KL2013G01);2013年湖北师范学院本科生科研立项项目(2013072)

摘　　要：目的合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮。方法采用一锅法Biginelli反应以乙酰乙酸乙酯、苯甲醛和尿素为原料,H3PW12O40/SiO2为催化剂,无水乙醇为溶剂进行合成目标化合物。通过熔点,IR,1 H NMR和MS等测试手段对合成的目标化合物进行表征。结果探讨了反应温度、催化剂用量、反应时间和反应物的摩尔比对收率的影响。实验表明:固定苯甲醛用量为0.04mol的条件下,催化剂的用量占反应物料总质量的2.0%,n(苯甲醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1∶1.5∶1.5,反应时间为90min,反应温度为90℃。在优化条件下,产品平均收率可达79.2%。结论溶胶凝胶法制备的H3PW12O40/SiO2是合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮的良好催化剂,具有催化剂用量少,催化活性高,可回收重复使用等特点。Objective--To synthesize 4-phenyl-6-methyl-5-ethoxycarbonyl-3, 4-dihydropyrimidin - 2 （H） -one. Methods--The target compound was synthesized via one-pot reaction with ethyl acetoace- tate, benzaldehyde and urea as raw materials, H3PW12040/SiO2 as catalyst and anhydrous ethanol as solvent. The 3, 4-dihydropyrimidin-2（H）-one were characterized by melting point measurements, IR, 1HNMR and MS spectroscopy. Results--The influence factors of reaction conditions on the yield of the target compound were discussed and the experiment showed that the best reaction were as fol- lows： under the condition of fixed benzaldehyde consumption is 0.04 tool, the anhydrous ethanol is 15 mL, the mass fraction of the catalyst to reactants is 2.0%, n （benzaldehyde） ： n （ethyl acetoacetate） ： n （urea） is 1 ： 1.5 ： 1.5, the reaction time is 90 min, and when the reaction temperature is 90 ℃, the yield of the product can reach 79.2%. Conclusion--The results indicate that the H3PW12040/SiO2, which was synthesized by a sol-gel technique, is a novel, effective and reusable catalyst for synthesi-zing 4-phenyl-6-methyl-5-ethoxycarbonyl-3, 4-dihydropyrimidin- 2（H）-one. The high activity and stability of the catalyst is well retained after 5 runs.

关 键 词：H3PW12O40/SiO2 3 4-二氢嘧啶酮 BIGINELLI反应 一锅法 

分 类 号：TQ426.91[化学工程]