双氢青蒿素制备工艺改进

以青蒿素为原料,硼氢化钠为还原剂,制备了双氢青蒿素。考察了溶剂选择及用量、还原剂用量、反应时间等因素对产物收率和质量分数的影响,优化的工艺条件为:当青蒿素用量1.5 g(5.31 mmol)时,反应温度0~5℃,甲醇溶剂用量100 mL,还原剂用量1.0 g(26.4 mmol),反应时间1.5 h,直接将反应液倒入250 mL冰冻去离子水中,过滤所得双氢青蒿素产物经UV、FTIR、HPLC和熔点测定进行了确证。与文献方法相比,该文报道工艺缩短了反应步骤和反应时间,收率从57.93%提高到71.54%,质量分数从99.33%提高到99.87%。

Improvement On Preparation Of Dihydroartemisinin

Dihydroartemisinin was prepared from artemisinin and sodium borohydride.The yield and purity of the product were taken for the observed indexes to analysis the influences of solvent choice,the amount of reductant and reaction time.The optimal reaction conditions were:the amount of artemisinin 1.5 g(5.31 mmol),reaction temperature 0 ℃ to 5℃,the amount of methanol solvent 100 mL,the amount of reductant 1.0 g(26.4 mmol)and reaction time 1.5 h.Then put the reaction liquid directly into 250 mL frozen deionized water and filtered to get dihydroartemisinin.The product was confirmed by UV,FTIR,HPLC and melting point.Compared with the literatures,not only the reaction step and reaction time are shortened,but also the yield and purity of the product obtained is improved from 57.93% and 99.33% to 71.54% and 99.87% respectively.