6-苯胺基-2-硫脲嘧啶合成工艺的优化  

Optimization of the Synthesis Process of 6-Anilino-2-Thiouracil

作　　者：李伟铭 康家铭 周芳 张志华[1] LI Wei-ming;KANG Jia-ming;ZHOU Fang;ZHANG Zhi-hua(College of Chemistry and Environmental Engineering,Liaoning University of Technology,Jinzhou Liaoning 121001,China)

机构地区：[1]辽宁工业大学化学与环境工程学院,辽宁锦州121001

出　　处：《辽宁化工》2021年第2期150-152,共3页Liaoning Chemical Industry

基　　金：国家级大学生创新创业项目(项目编号:201910154042);辽宁省自然科学基金指导计划项目(项目编号:2019-ZD-0693)。

摘　　要：以苯胺、氰乙酸乙酯、乙醇钠为原料经合环、胺置换反应合成6-苯胺基-2-硫脲嘧啶,并考察反应条件对产物收率的影响。结果表明:6-苯胺基-2-硫尿嘧啶合成的最佳工艺条件为:氰乙酸乙酯与硫脲物质的量之比为1∶1,回流反应3h,合环得到6-氨基-2-硫脲嘧啶;6-氨基-2-硫尿嘧啶、苯胺盐酸盐和苯胺物质的量之比为1∶2∶1,反应温度为170℃,微波反应时间为1.5 h;目标化合物反应总产率为80.70%,纯度可达99%以上。合成的化合物经1HNMR、13CNMR、HRMS等表征。Aniline, ethyl cyanoacetate and sodium ethoxide were used as raw materials to synthesize 6-anilino-2-thiouracil through ring closure and amine displacement reactions. The effect of reaction conditions on the yield of the product was investigated. The optimal process conditions for the synthesis of 6-anilino-2-thiouracil were determined as follows: the ratio of ethyl cyanoacetate to thiourea was 1 ∶ 1, and the reaction was refluxed for 3 h to obtain 6-amino-2-thiouracil;The ratio of the amount of 6-amino-2-thiouracil, aniline hydrochloride and aniline was 1∶2∶1, reaction temperature was 170℃, microwave reaction time was 1.5 h. Under above condition, total yield of target compound reaction was 80.70%, and the purity was more than 99%. The synthesized compound was characterized by 1HNMR, 13CNMR, HRMS and other patterns.

关 键 词：6-苯胺基-2-硫脲嘧啶 合成 工艺优化 

分 类 号：TQ254.1[化学工程—有机化工]