安吖啶合成工艺优化  

Optimization of Amsacrine Synthesis Process

作　　者：王宇斌 Wang Yu-bin

机构地区：[1]海南卓科制药有限公司,海南海口571127

出　　处：《化工设计通讯》2021年第12期44-44,171,共2页Chemical Engineering Design Communications

摘　　要：9-氯吖啶与3-甲氧-4-胺基-苯基甲磺酰胺发生亲核取代反应,碳酸氢钠为反应提供碱性条件,反应约4h,反应完成用水洗无机盐,再用乙酸乙酯作为析晶溶剂,制得抗肿瘤原料药安吖啶,再以N,N-二甲基乙酰胺重结晶,得到纯度较高的安吖啶,总收率为80%左右(以9-氯吖啶计),该工艺生产周期短、操作方便,不仅起始物料在市场上容易购买,生产过程中用到的溶剂均为普通易得,对人员、环境伤害性不大,安全风险较小,制备得到的产品纯度高,收率也很高。3-methoxy-4-amino-phenylmethanesulfonamide undergo a nucleophilic substitution reaction.Sodium bicarbonate provides basic conditions for the reaction.The reaction is about 4h.After the reaction is completed,the inorganic salt is washed with water.Then use ethyl acetate as the crystallization solvent to prepare the anti-tumor raw material amsacrine,and then recrystallize it with N,N-dimethylacetamide to obtain amsacrine with higher purity.The total yield is about 80%.(Calculated as 9-chloroacridine),the process has a short production cycle and convenient operation.Not only the starting materials are easy to buy in the market,but the solvents used in the production process are all common and easily available,and it is not harmful to personnel and the environment.,The solvent with less safety risk,the product obtained by the preparation has high purity,and the yield is also greatly improved.

关 键 词：安吖啶 合成 工艺优化 反应 时间 析晶 温度 

分 类 号：R914.5[医药卫生—药物化学]