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1-α-羟基苯乙酸拆分工艺研究

Improvement of resolution techniques of α-Hydroxybenzoic acid

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【作者】 熊正龙吴桂荣

【Author】 XIONG Zheng-long,WU Gui-rong(Department of Medicinal and Organic Chemistry,Xinjiang Medical University, Urumqi 830011,China)

【机构】 新疆医科大学药学院药化有机教研室

【摘要】 目的提高α-羟基苯乙酸的拆分效率。方法以右旋伪麻黄碱作为拆分剂,先与外消旋α-羟基苯乙酸反应,生成非对应异构体盐后,加入含钙、镁离子的沉淀剂,再进行分离纯化。结果 d-α-羟基苯乙酸收率为84.21%,光学纯度(OP)98.7%;1-α-羟基苯乙酸收率为91.1%,OP为85.1%,总收率为87.63%。拆分效率:d-α-羟基苯乙酸83.11%,1-α-羟基苯乙酸77.53%。结论加入含钙、镁离子的沉淀剂拆分d-α-羟基苯乙酸,光学纯度提高,工艺稳定。

【Abstract】 Objective To increase the separation efficiency of α-hydroxybenzoic acid.Methods D-pseudoephedrine as separation reagent was reacted with racemic α-hydroxybenzoic acid first,and then add precipitant which had calcium and magnesium after forming diastereoisomer salt and continue separated and purifid.Results Recovery rate of d-α-hydroxybenzoic acid was 84.21%,the optical purity(OP%) was 98.7%,l-α-hydroxybenzoic acid was 91.1%,optical purity(OP%) was 85.1%,the totalrecovery rate was 87.63%.Resolution efficiency of d-α-hydroxybenzoic acid,l-α-hydroxybenzoic acid was 83.11% and 77.53%,respectively.Cnclusion Adding calcium and magnesium ions to precipitating α-hydroxybenzoic acid had a high optical purity,and the chemical technology is stable.

【关键词】 α-羟基苯乙酸拆分沉淀剂
【Key words】 α-hydroxybenzoic acidresolutionprecipitant
  • 【文献出处】 新疆医科大学学报 ,Journal of Xinjiang Medical University , 编辑部邮箱 ,2012年01期
  • 【分类号】TQ245.12
  • 【被引频次】3
  • 【下载频次】76
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