依达拉奉合成工艺研究

Research on synthesis process of edaravone

提供了一种依达拉奉重结晶精制的方法。工业级依达拉奉为起始原料,无水乙醇为溶剂,活性炭为脱色剂,经高温溶解,热滤过炭,降温结晶得医药级依达拉奉成品。最佳工艺条件为依达拉奉、无水乙醇、活性炭质量比为1:1.25:0.0625,反应温度为80℃,反应时间为0.5 h,搅拌转速为200 r/min,降温至20℃,离心烘干即得依达拉奉产品。在重结晶过程中,依达拉奉的收率为84%。经高效液相色谱仪检测,依达拉奉产品的纯度为99.91%,单杂为0.04%,总杂为0.09%,符合中国药典2020年版的要求。

A method for recrystallization and refinement of edaravone was provided.Industrial grade edaravone is used as starting material,anhydrous ethanol as solvent,activated carbon as decolorizing agent,pharmaceutical grade edaravone finished product was obtained by high temperature dissolution,heat filtration of carbon,and cooling crystallization.The optimal process conditions were as follows:mass ratio of edaravone,anhydrant ethanol and activated carbon was 1:25:0.0625,reaction temperature was 80℃,reaction time was 0.5 h,stirring speed was 200 r/min,cooling to was 20℃,and edaravone products were obtained by centrifugal drying.During the recrystallization process,the yield of edaravone was 84%.After detection by high performance liquid chromatography,the purity of edaravone product was 99.91%,single impurity was 0.04%,total impurity was 0.09%,which meets the requirements of the Chinese Pharmacopoeia 2020 edition.