以磷酸为催化剂,在无溶剂条件下,通过芳香醛(1)、尿素(2)[或硫脲(3)]和乙酰乙酸乙酯的Biginelli缩合反应,合成了10个二氢嘧啶酮类化合物,其结构经1H NMR和IR表征.最佳反应条件:1 1 mmol,,n(1)∶n(2或3)∶n(乙酰乙酸乙酯)=1.0∶1.1∶1.0,于80℃反应15 min;于130℃反应25 min,产率80%~95%.与传统的Biginelli合成方法相比,该方法反应时间由18 h缩短至40 min,产率由20%~50%提高至80%~95%.
Ten 3,4-dihydropyrimidine-2 (1H)-ones were synthesized by the solvent-free Biginelli' s condensation of aldehyde ( 1 ), urea ( 2 ) [ or thiourea ( 3 ) ] and ethyl acetoacetate using phosphoric acid as the catalyst. The structure were characterized by 1H NMR and IR. The optimum reaction con- ditions at 80 ℃ for 15 rain and 130℃ for 25 rain were as follows: 1 was 1 mmol, n(1) : n(2 or 3) :n( ethyl acetoacetate) was 1.0 : 1.1 : 1.0. The yield was 80% ~ 95% under the optimum reac- tion conditions. The new synthetic method reduces the reaction time from 18 h to 40 min and en- hances the yields from 20% ~ 50% to 80% ~ 95%.