甘草次酸30位酰胺类衍生物的合成及结构表征

目的制备甘草次酸30位酰胺类衍生物—N-β-羟乙基30-甘草次酰胺并对其结构进行表征。方法以甘草次酸和2-氨基乙醇为原料,经碱催化缩合反应制备目标化合物;经光谱方法确定其化学结构;考察不同种类缩合剂、溶剂量、物料比、处理方法对目标化合物反应产率的影响,筛选最佳制备工艺。结果制备的甘草次酸30位酰胺类衍生物-N-β-羟乙基30-甘草次酰胺的产率为63%,并通过理化性质和光谱特征对其结构进行表征,对制备工艺进行优化。确定以EDCI、HOBt、DMAP为催化系统,催化量分别为起始原料甘草次酸的1.5倍、1倍和0.5倍,二氯甲烷为反应溶剂,反应时间为18h。结论优化的制备工艺操作简单,目标化合物产率高。

Synthesis and characterization of glycyrrhetinic acid 30-amined derivative

Objective To prepare and characterize glycyrrhetinic acid(GA) 30-amined derivative-glycyrrhetinic acid-30-hydroxyethyl amide(GA-HEA).Methods The base-catalyzed reaction of condensation was used for preparing target compound within GA and 2-aminoethanol as raw materials;spectrum methods were used for chemical structure determination;in parallel,the effects of different condensing agents,solvent quantity,ratio of reactants and treatment methods to the production yield were observed,the preparation techniques were investigated.Results The target compound glycyrrhetinic acid 30-N-β-hydroxyethyl amide was prepared with a yield of 63%;the spectrometric and physico-chemical properties were described;the preparation techniques were optimized.Conclusion The use of EDCI,HOBt and DMAP as catalyzing system for the condensation reaction with a ratio of 1.5,1 and 0.5 times towards the starting compound GA within 18 hours at room temperature,were the optimal reaction condition for preparing target compound within a relatively high yield.