摘要
本文开发了一种化合物N-(3,5-二氨基-6-氯吡嗪-2-甲酰基)硫脲(TM)的合成新工艺。将叔丁醇钾与硫脲原位反应制得硫脲钾盐,再与3,5-二氨基-6-氯-吡嗪甲酸甲酯发生亲核反应一步合成TM,收率85%,化学纯度99%,其结构经~1H NMR,^(13)C NMR和LC-MS表征。该合成工艺稳定,已放大至公斤级。
A new synthetic process of 1-（3,5-diamino-6-chloropyrazine-2-carbonyl）-thiourea（ TM ） was developed. TM in total yield of 85% and purity of 99% was prepared by only one step reaction of methyl 3,5-diamino-6- chloropyrazine-2-carboxylate with thiourea potassium salt which was obtained by in-situ reaction of thiourea with potassium tert-butoxide. The structure was confirmed by 1 H NMR, 13 C NMR and LC-MS. The process is stable and had been enlarged to kilogram scale production.
作者
朱剑平
余洛汀
林文清
ZHU Jian-ping;YU Luo-ting;LIN Wen-qing(State Key Laboratory of Biotherapy,Sichuan University,Chengdu 610041,China;Chengdu Porton Pharmaceutical Corporation Ltd.,Chengdu 610000,China)
出处
《合成化学》
CAS
CSCD
北大核心
2018年第9期699-702,共4页
Chinese Journal of Synthetic Chemistry
