一种强力霉素关键中间体的合成研究  

Synthesis of the key intermediate of doxycycline

作　　者：徐桂清 高原 吴斗灿 毛龙飞 姜玉钦 李伟 XU Gui-qing;GAO Yuan;WU Dou-can;MAO Long-fei;JIANG Yu-qin;LI Wei(School of Chemistry and Chemical Engineering,Henan Normal University,Henan Engineering Research Center ofChiral Hydroxyl Pharmaceutical,Collaborative Innovation Centre of Henan Province for Green Manufacturing of Fine Chemicals, Key Laboratory of Green Chemical Media and Reactions,Ministry of Ed;Hennan Ziweixing Chemistry Co.Ltd.,Xinxiang 4453011,China)

机构地区：[1]河南师范大学化学化工学院,河南省手性醇类药物工程技术研究中心,精细化学品绿色制造河南省协同创新中心,绿色化学介质与反应教育部重点实验室,河南新乡453007 [2]河南紫微星化学有限公司,河南新乡4453011

出　　处：《化学研究与应用》2018年第8期1354-1357,共4页Chemical Research and Application

基　　金：河南省科技创新杰出青年基金项目(164100510015)资助。

摘　　要：11α-氯代甲烯土霉素是合成强力霉素的关键中间体。本文以N-氯代乙酰苯胺和土霉素为起始原料,经氯代、脱水、成盐三步反应得到目标化合物,其结构经核磁共振氢谱、红外光谱确认,总收率达82.2%。本合成方法中所用新脱水剂的环境污染小、对设备腐蚀小、产品收率高,更适于工业化推广。The key intermediate of doxycycline,11α-chloro-metacycline,was synthesized from N-chloro acetanilide and oxytetracycline in three steps including chlorination,dehydration and salification.The structure of the intermediate was characterized by 1H NMR and HRMS.The overall yield of the synthetic route was 82.2%.The new dehydrant used in this method had the advantages of less pollution,lower corrosion and higher yield compared with anhydrous hydrogen fluoride,and it was more suitable for industrial application.

关 键 词：强力霉素 关键中间体 合成 

分 类 号：O621[理学—有机化学]