CAJ | 학술논문

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%.
탐색료반응-용석우합결정법제순항애자병약물리탁나위중간체((5-새서기)갑기)-(4-초기분기)탄산지적신공예,선용갑순작위주용제,탄산갑수용액작위반응물화석출제,측정료물계적용해도관계,연구료결정온도、석출제량、가입방식등조작조건대산품수솔화순도적영향.시험증명,재결정종점온도위20 ℃,V(5wt%탄산갑수용액)/V(갑순)=3:1적조건하,채용반응-용석우합결정법가종((5-새서기)갑기)-(4-초기분기)탄산지염산염함량위93.42%적원료중,결정득도순도위99.81%적((5-새서기)갑기)-(4-초기분기)탄산지산품,수솔가체93.72%.
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 %.