美沙拉嗪的合成工艺改进  

Improved Synthetic Process of Masalazine

作　　者：张文雯[1] 翁智兵 巩冰倩 王聿鹏 叶爱英[1] ZHANG Wenwen;WENG Zhibing;GONG Bingqian;WANG Yupeng;YE Aiying(School of Chemical and Pharmaceutical Engineering,Changzhou Institute of Engineering Technology,Changzhou 213164)

机构地区：[1]常州工程职业技术学院化工与制药工程学院,江苏常州213164

出　　处：《中国医药工业杂志》2020年第9期1136-1138,共3页Chinese Journal of Pharmaceuticals

摘　　要：以对硝基苯酚为起始原料,经Duff醛基化、在溴化铜/叔丁基过氧化氢/叔丁醇钾条件下氧化、氯化亚锡/浓盐酸体系中还原得到目标化合物美沙拉嗪,总收率为54%,化合物结构经IR、~1H NMR表征。在Duff醛基化反应过程中,采用对甲苯磺酸为催化剂,简化了操作,收率由文献的67%提高至93%。整条路线操作简单,适合工业化生产。Masalazine in a total yield of 54% was obtained via three steps of improved Duff formylation,oxidization in presence of CuBr2/TBHP/t-BuOK,and reduction in the SnCl2/HCl system,from p-nitrophenol as starting material.The structures of intermediates and product were characterized by IR and 1H NMR.p-TSOH used in the process of Duff formylation not only simplified the operation steps,but also improved the yield to 93%,higher than that reported in the literature(67%).The whole route was easy to operate and suitable for industrial production.

关 键 词：美沙拉嗪 抗结肠炎药物 Duff醛基化 氧化 还原 

分 类 号：TQ246.3[化学工程—有机化工] R975[医药卫生—药品]