一种低成本高含量曲克芦丁的制备方法  

A preparation method of low cost and high content of troxerutin

作　　者：李阳 郭利兵[2] 谷少华[3] 李言言 毛龙飞 李星 曹晓慧 张玮玮 李伟 姜玉钦 LI Yang;GUO Li-bing;GU Shao-hua;LI Yan-yan;MAO Long-fei;LI Xing;CAO Xiao-hui;ZHANG Wei-wei;LI Wei;JIANG Yu-qin(Henan Engineering Research Center of Chiral Hydroxyl Pharmaceutical,School of Chemistry and Chemical Engineering,Henan normal university,Xinxiang 453007,China;Institute of Chemistry,Henan Academy of Sciences,Zhengzhou 450002,China;Xinxiang Central Hospital,Xinxiang 453000,China)

机构地区：[1]河南师范大学化学化工学院,河南省手性醇类药物工程技术研究中心,河南新乡453007 [2]河南省科学院化学研究所有限公司,河南郑州450002 [3]新乡市中心医院,河南新乡453000

出　　处：《化学研究与应用》2019年第6期1073-1078,共6页Chemical Research and Application

基　　金：河南省杰出青年创新人才项目(174100510025)资助

摘　　要：本文以市售芦丁为原料,在吡啶中经醋酸酐酰化后再水解得外标含量为99.7%的高纯度芦丁;然后以此高纯度芦丁为原料,以3代聚酰胺-胺树枝状聚合物为催化剂,在甲醇中经环氧乙烷羟乙基化反应,精制后得高含量曲克芦丁。本文系统研究了以高纯度芦丁为原料,反应温度、时间和压强对曲克芦丁合成的影响。实验表明,芦丁经酰化后再水解可得到纯度为99.7%的高纯度芦丁,在高压釜内,压强0.2MPa、温度80℃条件下反应5 h,得到的粗品曲克芦丁只需简单纯化便可得到外标纯度大于98.5%的曲克芦丁。The high-purity rutin(over 99.7%),which were obtained through acetylation of rutin by acetic anhydride in pyridine and then hydrolysis of the acylated rutin by sodium methoxide in methanol,could be used as the starting materials to produce the high-content troxerutin by etherification using the three generations of polyamidoamine dendrimers as catalyst and ethylene oxide as the hydroxyethylation reagent.After optimized the reaction conditions such as reaction temperature,time and pressure,the high-purity troxerutin(over 98.5%)could be obtained using the high-purity rutin(99.7%)as the starting materials by simple purification.The optimized reaction time was 5 hours under 0.2 MPa pressure at 80℃.

关 键 词：3代树枝状聚酰胺-胺 芦丁 曲克芦丁 

分 类 号：O633.22[理学—高分子化学]