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出 处:《化工时刊》2004年第10期22-24,共3页Chemical Industry Times
摘 要:介绍了 2 -氯嘧啶的合成工艺路线 ,研究了多种因素对每步反应收率的影响 ,得到较佳的工艺条件。实验结果表明丙二酸二乙酯和盐酸胍反应以 4h为佳 ,合成的 4 ,6 -二羟基 - 2 -氨基嘧啶以二氯甲烷为溶剂反应得 4 ,6 -二氯- 2 -氨基嘧啶 ,脱氯反应的较佳配比为n(Na)∶n(Zn)∶n(4,6 -二氯 - 2 -氨基嘧啶 ) =2 .6∶3∶1,合成 2 -氯嘧啶的较佳原料配比为n(2 -氨基嘧啶 )∶n(ZnCl2 )∶n(NaNO2 ) =1∶3∶1.7,反应总收率为 4 3.7%。A preferable method of preparing 2-chloropyrimidine was introduced in this article.Experiments were done under different conditions of reaction,and the optimal conditions to synthesis of 2-chloropyrimidine were obtained.The most suitable conditions for the synthesis were as follows:the reaction time to prepare 4,6-dihydroxyl-2-aminopyrimidine from diethyl malonate and guanidine hydrochloride was 4h,the solvent used to prepare 4,6-dichloro-2-aminopyrimidine from the former intermediate was methylene chloride, the mole ratio of dehydrochlorination of Na∶Zn∶4,6-dichloro-2-aminopyrimidine was 2.6∶3∶1 and in the last step the mole ratio of 2-aminopyrimidine :ZnCl 2∶NaNO 2 was 1∶3∶1.7.The total yield is over 43.7%.
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