硬脂醇甘草亭酸酯绿色合成工艺  

Research on green synthesis process of stearyl glycyrrhizinate

作　　者：汪洋 程建明 阚建伟 季浩[2] WANG Yang;CHENG Jian-ming;KAN Jan-wei;JI Hao(School of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210023,China;Jiangsu Tiansheng Pharmaceutical Co.Ltd,zhenjiang 212415,China)

机构地区：[1]南京中医药大学药学院,江苏南京210023 [2]江苏省天晟药业股份有限公司,江苏镇江212415

出　　处：《化学研究与应用》2024年第3期681-688,共8页Chemical Research and Application

基　　金：国家重点研发计划“战略性国际科技创新合作”重点专项项目(2018YFE0208600)资助。

摘　　要：探索硬脂醇甘草亭酸酯的较优合成条件,为甘草资源的合理开发利用提供依据。采用高效液相色谱法(HPLC)检测硬脂醇甘草亭酸酯的纯度,以硬脂醇甘草亭酸酯的纯度和产率为指标,在单因素实验的基础上,设计正交试验对硬脂醇甘草亭酸酯合成工艺进行优化。本实验得出硬脂醇甘草亭酸酯的最佳合成工艺参数为:以无水碳酸钾作为催化剂,甘草次酸、1-溴十八烷和无水碳酸钾的投料摩尔比为1:1.5:2、反应时间为3h、反应温度为70℃;在此条件下,所得硬脂醇甘草亭酸酯的纯度为98.52%,产率为87%,样品结构经IR、MS、^(1)H NMR确证,质量符合现有硬脂醇甘草亭酸酯质量标准。本实验所得硬脂醇甘草亭酸酯合成工艺具有操作步骤少、三废排放量少、能源消耗少等特点,具有绿色环保的优势,合成的目标产物硬脂醇甘草亭酸酯有望成为中草药化妆品配伍组分的重要来源。In order to rational development and utilization of Glycyrrhiza uralensis Fisch,the synthesis conditions of stearyl glycyrrhizinate were explored.Here the purity and yield of stearyl glycyrrhizinate were used as indicators which detected by high performance liquid chromatography(HPLC) to optimize the synthesis process of stearyl glycyrrhizinate.With the basic of single-factor experiment,the synthesis process of stearyl glycyrrhizinate was optimized via the orthogonal test.In this experiment,the optimal synthesis process parameters of stearyl glycyrrhizinate were as follows:anhydrous potassium carbonate was used as catalyst,and the molar ratio of glycyrrhetinic acid,1-bromooctadecane and anhydrous potassium carbonate was 1:1.5:2,reaction time was 3 h,reaction temperature was 70℃;Under these conditions,the purity of stearyl glycyrrhizinate was 98.52%and the yield was 87%.The sample structure was identified by IR,MS,^(1)H NMR,and the quality conformed to the existing quality standards of stearyl glycyrrhizinate.The synthesis process of stearyl glycyrrhizinate obtained in this study was green with the advantages of fewer operation steps,less emissions of three wastes and less energy consumption.The target product,stearyl glycyrrhizinate,would contribute to the important source of components of Chinese herbal cosmetics.

关 键 词：硬脂醇甘草亭酸酯 合成 单因素实验 正交试验 

分 类 号：O623.624[理学—有机化学]