7-氨基-3-甲氧基甲基-3-头孢烯-4-甲酸的合成  

Synthesis of 7-amino-3-methoxymethyl-3-cephem-4-carboxylic acid

作　　者：孙美婷 姜鹏鹏 梁丙辰 王宇栋 Sun Meiting;Jiang Pengpeng;Liang Bingchen;Wang Yudong(Hejia Research Institute,Hebei Hejia Pharmaceutical Science and Technology Group,Shijiazhuang 050000,China)

机构地区：[1]河北合佳医药科技集团合佳研究院

出　　处：《煤炭与化工》2019年第11期126-131,160,共7页Coal and Chemical Industry

摘　　要：7-氨基-3-甲氧基甲基-3-头砲烯-4-甲酸(7-AMCA)是头砲泊岳酯合成的必备中间体。针对目前以7-氨基头胞烷酸(7-ACA)或D-7-ACA为起始原料合成7-AMCA的2种工艺路线均存在工艺条件苛刻、溶剂难回收、环保压力大、产品纯度低等缺陷,为了开发1种适合其工业生产的绿色制备工艺,在以D-7-ACA制备7-AMCA的基础上,通过实验考察了关键原材料的用量、反应温度、反应时间等对产品收率及质量的影响。实验结果表明,当反应温度为30℃,反应时间为15 min,原料原甲酸三甲酯与D-7-ACA的物质的量比为2:1,氨水作为碱性析晶试剂时,制得的7-AMCA产品性状好、纯度高,该工艺更有利于工业化生产。7-Amino-3-methoxymethyl-3-cephem-4-carboxylic acid(7-AMCA)is an essential intermediate for the synthesis of cefpodoxime proxetil.At present,the two processes for synthesizing 7-AMCA with 7-amino cefalic acid(7-ACA)or D-7-ACA as raw materials all have defects such as harsh process conditions,difficult solvent recovery,high environmental pressure and low product purity.In order to develop a green preparation process suitable for its industrial production,based on the preparation of 7-AMCA by D-7-ACA,the effects of key raw material dosage,reaction temperature and reaction time on product yield and quality were investigated through experiments.The experimental results show when the reaction temperature is 30℃ and the reaction time is 15 min,the ratio of the raw material of trimethyl orthoformate to D-7-ACA is 2:1,and ammonia is used as the basic crystallization reagent,the obtained 7-AMCA has good properties and high purity,and the process is more conducive to industrial production.

关 键 词：7-AMCA D-7-ACA 甲烷磺酸 原甲酸三甲酯 

分 类 号：TQ463.25[化学工程—制药化工]