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目的对甘草萜醇类共轭烯衍生物—11-脱氧-11,13(18)-二烯甘草萜醇的合成工艺进行优化及结构表征。方法以甘草次酸为原料,分别用红铝和硼氢化钠-碘体系进行还原修饰制得目标化合物,对2种方法的工艺和产率进行考察;用常规的四大光谱法确定化学结构。结果用红铝经两步反应制得目标化合物的总产率为29%;用硼氢化钠-碘体系还原可用一步制得目标产物,产率达65%。经第2种方法简化了操作流程,优化了纯化工艺;详细描述了目标化合物的光谱特征和理化性质。结论用硼氢化钠-碘体系还原制备11-脱氧-11,13(18-)二烯甘草萜醇的操作简单,产率高,是制备甘草萜醇类共轭双烯衍生物的较好途径。
OBJECTIVE To optimize and characterize the synthesis of glycyrrhizin alcohol conjugated conjugated diene derivative-11-deoxy-11,13 (18) -diene licoricetiol. Methods Glycyrrhetinic acid was used as raw material, and the target compounds were prepared by reductive modification with red aluminum and sodium borohydride - iodine respectively. The process and yield of the two methods were investigated. The chemical structure was determined by four conventional spectroscopy methods. Results The total yield of the target compound obtained by two steps reaction of red aluminum was 29%. The target product was obtained in one step by reduction with sodium borohydride - iodine. The yield was 65%. The second method simplifies the operation process and optimizes the purification process. The spectral characteristics and physicochemical properties of the target compounds are described in detail. Conclusion The reduction of 11-deoxy-11,13 (18-) diketopyrl alcohol by sodium borohydride-iodine system is simple and the yield is high. It is a good way to prepare the conjugate diene derivatives of glymetinol .