摘要
以利福霉素S、液溴、2-氨基-4-甲基吡啶、抗坏血酸(VC)为主要原料,经过溴化、环合、还原三个步骤制备了利福昔明。结果表明,最优工艺条件为:溴化反应采用乙醇和水溶剂体系,利福霉素S与溴的摩尔比为1∶1.2;环合反应中3-Br-利福霉素S与2-氨基-4-甲基吡啶的摩尔比为1∶1.6,反应温度为63℃。在该优化条件下,产品总收率达85.1%。
In this paper, rifaximin was prepared with rifamycin S, bromine, 2-amino-4-methylpyridine and vitamin C as the main raw material, via three steps of bromination, cyclization and reduction. The result showed that the optimum reaction conditions were determined as follows： In reduction, the solvent was ethanol/water and the molar ratio of rifamycin S to bromine of 1 ∶1.2. In cyclization, the molar ratio of rifamycin S to 2-amino-4-methyl-pyridine of 1∶1.6 and the reaction temperature is 60 ℃. Under the optimum condition, the yield of the product reached 85.1%.
出处
《浙江化工》
CAS
2016年第8期21-24,54,共5页
Zhejiang Chemical Industry
关键词
利福昔明
合成
工艺优化
rifaximin
synthesis
process optimization
