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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。
Objective To prepare the 30-glycyrrhetinic acid amide derivative of glycyrrhetic acid 30 and characterize its structure. Methods Glycyrrhetinic acid and 2-aminoethanol were used as starting materials to prepare the target compounds by alkali-catalyzed condensation reaction. The chemical structures of the target compounds were determined by spectroscopic methods. The effects of different types of condensing agents, solvent amount, material ratio and treatment methods on the yield of target compounds The impact of screening the best preparation process. Results The yield of N-β-hydroxyethyl 30-glycyrrhetinic acid amide was 30%. The yield of glycyrrhetinic acid derivative was 63%. Its structure was characterized by its physicochemical properties and spectral characteristics, and the preparation process was optimized . Determined to EDCI, HOBt, DMAP as the catalytic system, the catalytic amount of glycyrrhetinic acid as the starting material were 1.5 times, 1 times and 0.5 times, dichloromethane as the reaction solvent, the reaction time was 18h. Conclusion The optimized preparation process is simple and the yield of target compound is high.