正交设计优选微波辐射下依达拉奉的合成条件

Optimization the Synthesis Conditions of Edaravone under Microwave Irradiation by Orthogonal Design

目的：以微波辐射法合成依达拉奉,并利用正交设计法探索微波辐射合成依达拉奉的最佳反应条件。方法：以反应原料比、反应溶剂量和反应时间为三个因素,采用L9（34）试验方案,通过直观分析和方差分析筛选出最佳反应条件。结果优选出的合成条件为苯肼：乙酰乙酸乙酯1∶1,乙醇12.5m L（苯肼为0.1m L时）,微波辐射反应12.5min,按上述最佳反应条件重复实验,所得结果稳定,将传统的3~5h缩短至12.5min,收率提高至37%以上。结论：该条件极大地缩短了反应时间,降低了能耗,绿色环保,符合绿色发展。

Objective： To optimize the Synthesis Conditions of Edaravone under Microwave Irradiation by Orthogonal Design Method： The ratio of reactants,solvent volume and heating time as the three factors,using orthogonal design method of L_9（ 3~4） test,and use the intuitive analysis and variance analysis to filter out the best reaction conditions. Results： The optimized synthesis conditions： Phenylhydrazine： ethyl acetoacetate = 1∶ 1,ethanol 12. 5m L（ when Phenylhydrazine is 0. 1m L）,time of microwave radiation is 12. 5min. According to the conditions,the experiments repeated many times,and the results showed stability and highest yield. Conclusion： The Synthesis time is shortened from 3 ~ 5h to 12. 5min,the yield increase to 37%,which not only greatly shorten the reaction time,but also decrease the reaction energy,with green environmental protection,green development.