摘要
以乙酰乙酸乙酯和尿素为原料,用对甲苯磺酸作催化剂合成6-甲基尿嘧啶,探讨了不同相转移催化剂、带水剂、相转移催化剂用量及脱水缩合时间等因素对反应产物产率的影响。得出最佳工艺条件为:19.8m L乙酰乙酸乙酯、10g尿素,对甲苯磺酸1.2g,150m L石油醚作带水剂,0.3g聚乙二醇200作相转移催化剂,回流脱水缩合8h,产率可达78%。
6-meyhyl uracil was synthesized from ethyl acetoacetate and urea with p-toluenesulfonic acid as catalyst. The effects of phase transfer catalysts,water-carrying agents,amount of phase transfer catalyst and reaction time on yield of 6-meyhyl uracil were studied. The optimum conditions were as follows: fixed ratio of raw materials n( urea) ∶ n( ethylacetoacetate) = 0. 167 mol ∶ 0. 157 mol = 1. 06 ∶ 1,the amount of p-toluenesulfonic acid 1. 2g;150m L petroleum ether as water-carrying agent; 0. 3g polyethylene glycol 200 as phase transfer catalyst; reaction time 8h; and reaction temperature 72℃,the yield of 6-meyhyl uracil was 78%.
出处
《合成材料老化与应用》
2015年第1期71-73,共3页
Synthetic Materials Aging and Application
基金
河南省重点科技攻关项目(132102210263)
河南省科技计划项目(122102210426)