H4SiW12O40/SiO2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
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TQ426.91

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2013年国家级大学生创新创业训练计划项目(201313256001)和湖北师范学院硕士研究生创新科研基金项目(1051320130216)


One-pot Synthesis of 4-Phenyl-6-Methyl- 5-Ethoxycarbonyl -3,4-Dihydropyrimidin-2(H)-one with H4SiW12O40/SiO2
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    摘要:

    采用一锅法Biginelli反应以H4SiW12O40/SiO2为催化剂,苯甲醛,乙酰乙酸乙酯和尿素为原料,无水乙醇为溶剂合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮。探讨了原料物质的量比、反应温度、催化剂用量及反应时间对收率的影响。实验表明:固定苯甲醛用量为0.04mol的条件下,n(苯甲醛):n(乙酰乙酸乙酯): n(尿素)=1:1.5:1.5,催化剂的用量占反应物料总质量的2.0%,反应温度为90℃,反应时间为60min。在优化条件下,产品平均收率可达71.7%。通过熔点的测定,IR,1H NMR和MS等对合成的3,4-二氢嘧啶酮化合物进行了表征。

    Abstract:

    H4SiW12O40/SiO2 exhibited excellent catalytic for synthesis of 4-Phenyl-6-Methyl-5-Ethoxycarbonyl -3,4-Dihydro -pyrimidin-2(H)-one via one-pot Biginelli reaction from benzaldehyde, ethyl acetoacetate, urea and anhydrous ehanol as soivent.The effects of reaction on the yield of the product were investigated and the optimum conditions were determined as follows: under the condition of fixed benzaldehyde consumption is 0.04mol n(benzaldehyde):n(ethylacetoacetate):n(urea)= 1:1.5:1.5,the quantity of catalyst was 2.0% quantity of the feed stock , reaction temperature was 90℃, and reaction time was 1.0h .The yield of the product was up to 71.7%.The 3,4-Dihydropyrimidin-2(H)-one were characterized by melting point measure ments,IR 1HNMR and MS spectroscopy.

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龚文朋,向诗银,杨水金,徐玉林. H4SiW12O40/SiO2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[J].精细化工,2014,31(2):

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  • 收稿日期:2013-10-16
  • 最后修改日期:2013-11-20
  • 录用日期:2013-11-21
  • 在线发布日期: 2014-01-03
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