二氧化硅负载磷钨酸催化合成3,4-二氢嘧啶-2(1H)-酮衍生物

doi:10.3724/SP.J.1095.2014.40046

摘要/Abstract

摘要： 以取代苯甲醛、乙酰乙酸乙酯和尿素为原料，以溶胶凝胶法制备二氧化硅负载的磷钨酸（H3PW12O40/SiO2）为催化剂，催化合成3,4-二氢嘧啶-2(1H)-酮，考察了三组分摩尔比、反应温度、催化剂用量及反应时间对反应收率的影响。研究表明，H3PW12O40/SiO2是合成3,4-二氢嘧啶-2(1H)-酮的良性催化剂，在取代苯甲醛的用量为0.04 mol，反应温度为90 ℃的条件下，收率可达73.1%~88.4%。催化剂和产品结构分别经IR、XRD、SEM和1H NMR、IR、MS等技术手段表征。

关键词: 溶胶凝胶法, 磷钨酸/二氧化硅, 催化, 合成, 二氢嘧啶-2(1H)-酮

Abstract: 3,4-Dihydropy-rimidine-2(1H)-one was synthesized from substituted benzaldehyde, ethylacetoacetate and urea using phosphotungstic acid（H3PW12O40） supported on SiO2 as a novel eco-friendly catalyst prepared by a sol-gel technique. The influences of the molar ratio of reactants, reaction temperature, catalyst loading and reaction time were discussed. H3PW12O40/SiO2 is a good catalyst for the synthesis of 3,4-dihydropy-rimidine-2(1H)-one with the yield of 73.1%~88.4% under optimized conditions. The catalyst was characterized by IR, XRD and SEM, and the products were characterized by 1H NMR, IR and MS.

Key words: sol-gel technique, phosphotungstic acid/silica, catalysis, synthesis, dihydro-pyrimidine-2(1H)-one

中图分类号:

徐玉林, 龚文朋, 杨水金. 二氧化硅负载磷钨酸催化合成3,4-二氢嘧啶-2(1H)-酮衍生物[J]. 应用化学, DOI: 10.3724/SP.J.1095.2014.40046.

XU Yulin, GONG Wenpeng, YANG Shuijin*. Synthesis of 3,4-Dihydropyrimidine-2(1H)-one Derivatives Using Phosphotungstic Acid Supported on Silica as Catalyst[J]. Chinese Journal of Applied Chemistry, DOI: 10.3724/SP.J.1095.2014.40046.

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