H_4SiW_6Mo_6O_(40)/SiO_2促进一锅法合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮  

One-pot Synthesis of 4-Phenyl-6-Methyl-5-Ethoxycarbonyl-3,4-Dihydropyrimidin-2(H)-one with H_4SiW_6Mo_6O_(40)/SiO_2

作　　者：杨水金[1] 徐玉林[1] 龚文朋[1] 喻莉[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：《徐州工程学院学报（自然科学版）》2014年第2期11-16,共6页Journal of Xuzhou Institute of Technology(Natural Sciences Edition)

基　　金：2013年湖北师范学院硕士研究生创新科研基金(1051320130216);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)

摘　　要：采用溶胶-凝胶法制备H4SiW6Mo6O40/SiO2为催化剂,以乙酰乙酸乙酯、苯甲醛和尿素为原料,无水乙醇为溶剂一锅法合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮.研究结果表明:催化剂用量、反应温度、反应时间和反应物的物质的量比是影响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)为1∶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2.5%,反应时间为90min时,产品收率可达72.3%.通过熔点,IR,1HNMR和MS等测试手段对合成的3,4-二氢嘧啶酮化合物进行了表征.A new catalyst,H4SiW6Mo6O40/SiO2was prepared by a sol-gel technique.Using H4SiW6Mo6O40/SiO2as catalyst,4-phenyl-6-methyl-5-ethoxycarbonyl-3,4-dihydropyrimidin-2-（H）-one was synthesized via one-pot method reaction from ethyl acetoacetate,with benzaldehyde,urea and anhydrous ethanol as solvent.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 is 0.04mol and anhydrous ethanol is 15mL,n（benzaldehyde）：n（ethylacetoacetate）：n（urea）is 1∶1.2∶1.5,reaction temperature is 90℃,mass fraction of catalyst to reactants is 2.5%and reaction time is 90min.The yield of the product can reach 72.3%.The 3,4-dihydropyrimidin-2（H）-one was characterized by melting point measurements,IR,HNMR and MS spectroscopy.

关 键 词：H4SiW6Mo6O40/SiO2 嘧啶酮 溶胶-凝胶法 一锅法 

分 类 号：TQ426.91[化学工程]