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机构地区:[1]河南师范大学化学与环境科学学院,新乡453007
出 处:《应用化学》2009年第10期1206-1210,共5页Chinese Journal of Applied Chemistry
基 金:河南省教育厅自然科学基金(2006530008)资助项目
摘 要:以FeCl3.6H2O为催化剂,无水乙醇为溶剂,n(取代-4-甲酰基吡唑)∶n(乙酰乙酸乙酯)∶n((硫)脲)∶n(FeCl3).n(6H2O)=1∶3∶3∶1,采取微波辐射和常规加热回流的方法,通过Biginelli缩合反应一锅合成了6种新型含吡唑基的3,4-二氢嘧啶类化合物,并进行了元素分析、IR、1H NMR和13C NMR表征,对反应机理和化合物的图谱特征进行了探讨。结果表明,利用微波辐射法合成含吡唑基3,4-二氢嘧啶类化合物具有反应时间短,产率高等优点。Pyrazol-3,4-dihydropyrimidines were synthesized by one-pot Biginelli cyclocondensation of substituted-4-formylpyrazole, ethyl acetoacetate, urea or thiourea and ferric choride ( in molar ratio of 1 : 3: 3: 1 ) in ethanol, under traditional heating or microwave irradiation conditions, while ferric chloride was used as a catalyst. The structures of all the products were characterized by elemental analysis, IR, ^1H NMR and ^13C NMR. The mechanism of the reaction and the spectra of all the compounds were also discussed. The method of microwave irradiation showed some advantages, such as a shorter reaction time and a higher yield, which is a new approach for synthesizing this kind of compounds.
关 键 词:三氯化铁 Biginelli缩合反应 二氢嘧啶 一锅合成 微波辐射
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