CAJ | 학술논문

研究了重要的医药中间体嘧啶的合成工艺,以尿素和丙二酸二乙酯为原料,在甲醇钠催化下合成巴比妥酸,并用三氯氧磷在N,N-二甲基苯胺催化下加氯成2,4,6-三氯嘧啶,将2,4,6-三氯嘧啶以钯碳催化,加氢脱氯得到嘧啶.得出每一步的最佳工艺条件,巴比妥酸合成:配料摩尔比1:1.1:1.2(丙二酸二乙酯:尿素:甲醇钠),回流,2 h;2,4,6-三氯嘧啶合成:配料摩尔比5:1(三氯氧磷:巴比妥酸),100～105℃,2 h;嘧啶合成:配料摩尔比5:1(氧化镁:2,4,6-三氯嘧啶),溶剂体积比3:1(水:乙醇),0.1 MPa,14 h,60℃.
연구료중요적의약중간체밀정적합성공예,이뇨소화병이산이을지위원료,재갑순납최화하합성파비타산,병용삼록양린재N,N-이갑기분알최화하가록성2,4,6-삼록밀정,장2,4,6-삼록밀정이파탄최화,가경탈록득도밀정.득출매일보적최가공예조건,파비타산합성:배료마이비1:1.1:1.2(병이산이을지:뇨소:갑순납),회류,2 h;2,4,6-삼록밀정합성:배료마이비5:1(삼록양린:파비타산),100～105℃,2 h;밀정합성:배료마이비5:1(양화미:2,4,6-삼록밀정),용제체적비3:1(수:을순),0.1 MPa,14 h,60℃.
The new process of preparing pyrimidine which is widely used as pharmaceutical intermediate was studied. Beginning from the raw material-- urea and diethyl malonate, barbituric acid was prepared with sodium methoxide as catalyst, then 2,4,6-trichloropyrimidine was synthesized by reacting of barbituric acid with phosphorus oxychloride in the presence of N,N-dimethylaniline. The object compound was prepared from 2,4,6-trichloropyrimidine by catalytic hydrogenation with palladium-charcoal as catalyst. The optimum reaction conditions for every reaction step were studied. For preparing barbituric acid, the mole ratio of diethyl malonate, urea and sodium methoxide was 1 : 1.1 : 1.2, and the mixture was refluxed 2 hours; for preparing 2,4,6-trichloropyrimidine, the mole ratio of phosphorus oxychloride and barbituric acid was 5 : 1, and the reaction was run at 100 - 105 ℃ for 2 hours; for preparing pyrimidine, the mole ratio of magnesium oxide and 2,4,6-trichloropyrimidine was 5 :1, the volume ratio of water and ethanol was 3 : 1 and the reaction was run at 0. 1 Mpa and 60 ℃ for 14 hours.