反应-溶析耦合结晶法提纯（（5-噻唑基）甲基）-（4-硝基苯基）碳酸酯

探索了反应-溶析耦合结晶法提纯抗艾滋病药物利托那韦中间体((5-噻唑基)甲基)-(4-硝基苯基)碳酸酯的新工艺,选用甲醇作为主溶剂,碳酸钾水溶液作为反应物和析出剂,测定了物系的溶解度关系,研究了结晶温度、析出剂量、加入方式等操作条件对产品收率和纯度的影响.试验证明,在结晶终点温度为20 ℃,V(5wt%碳酸钾水溶液)/V(甲醇)=3:1的条件下,采用反应-溶析耦合结晶法可从((5-噻唑基)甲基)-(4-硝基苯基)碳酸酯盐酸盐含量为93.42%的原料中,结晶得到纯度为99.81%的((5-噻唑基)甲基)-(4-硝基苯基)碳酸酯产品,收率可达93.72%.

Purification of((5-Thiazoyl)methyl)-(4-nitrophenyl) Carbonate by Coupling of Reaction and Solvating-out Crystallization

A new separation process, coupling of reaction and solvating-out crystallization, to purify ((5-thiazoyl) methyl)-(4-nitrophenyl) carbonate was explored. The effect factors such as crystallization temperature, quantity of anti-solvent and the feed method on the purity and yield of the product were studied.Methanol was used as solvate, aqueous potassium carbonate was used as reactant and precipitation agent. The result showed when the terminal cooling temperature was 20 ℃, 5wt% aqueous potassium carbonate/ methanol(v/v) was 3:1, product purity could attain 99.81% from raw material whose purity was 93.42% and the yield could reach 93.72 %.