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

摘要探索了反应-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)碳酸酯的工艺过程。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、析出剂量和加入方式等操作条件对产品收率和纯度的影响。试验表明,在结晶终点温度为20℃,V〔碳酸钾水溶液(质量分数5.0%)〕/V(甲醇)=3.0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)碳酸酯盐酸盐质量分数为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%。

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	石滨
	张国亮
	张凤宝

关键词：溶析结晶利托那韦耦合中间体

Abstract： This paper is to explore a new separation process,to purify((5-thiazoyl)methyl)-(4-nitrophenyl) carbonate by coupling of reaction and solvating-out crystallization.The effects,such as crystallization temperature,quantity of anti-solvent and the feed method on the purity and yield of the product were analyzed.The solubility of system was determined when methanol was used as solvate,aqueous potassium carbonate was used as reactant and precipitation agent.The results show,when the terminal cooling temperature is 20 ℃,5% aqueous potassium carbonate/methanol(V/V) is 3∶1,by the new separation process,the purity of product could attain 99.81% from raw material with purity of 93.42% and the yield could reach 93.72%.

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Received 2009-03-15; published 2009-03-15

引用本文:

石滨;张国亮;张凤宝;.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[J]. 化学工业与工程, 2009,26(2): 103-108

SHI Bin,ZHANG Guo-liang,ZHANG Feng-bao.Coupling of Reaction and Solvating-out Crystallization to Purify ((5-thiazoyl) methyl)-(4-nitrophenyl) Carbonate[J]. Chemcial Industry and Engineering, 2009,26(2): 103-108

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