以FeCl_3·6H_2O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(FeCl_3)·n(6H_2O)=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~(13)C 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 ~(13)C 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.
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