二苯甲酮腙电氧化制备二苯重氮甲烷的研究  

Study on Electrooxidation of Benzophenone Hydrazone to Diphenyldiazomethane

作　　者：韩璐瑶 胡硕真 郭庆春 郭红永 高照群 许颖 张新胜[1] Han Luyao;Hu Shuozhen;Guo Qingchun;Guo Hongyong;Gao Zhaoqun;Xu Ying;Zhang Xinsheng(School of Chemical Engineering,East China University of Science and Technology,Shanghai 200237;Hebei Lansheng Biotech Co.,Ltd.,Shijiazhuang,Hebei 052260)

机构地区：[1]华东理工大学化工学院,上海200237 [2]河北兰升生物科技有限公司,河北石家庄052260

出　　处：《有机化学》2024年第3期951-965,共15页Chinese Journal of Organic Chemistry

摘　　要：研究了二苯甲酮腙电催化氧化合成二苯重氮甲烷.针对二苯重氮甲烷的不稳定特性,通过非均相电解体系设计,优选卤化合物、电解质种类、反应溶剂的极性以及电极材料、控制电流密度和反应温度等措施,抑制过氧化副产物二苯甲酮、水解副产物二苯甲醇及偶联副产物二苯甲酮吖嗪的生成,以74%的高收率获得二苯重氮甲烷.此外,还初步探究了二苯甲酮腙电氧化机理.The electrocatalytic oxidation of benzophenone hydrazone for the synthesis of diphenyldiazomethane was investigated.To address the instability of diphenyldiazomethane,a heterogeneous electrolytic system was designed,optimizing the halogen compound,electrolyte type,solvent polarity,electrode material,control current density and reaction temperature.These measures effectively suppressed the formation of by-products such as benzylidene acetone peroxide,diphenylmethanol hydrolysis,and diphenylmethanequinone coupling,leading to a high yield of 74%for diphenyldiazomethane.Additionally,preliminary investigations were conducted on the electrochemical oxidation mechanism of benzophenone hydrazone.

关 键 词：间接电合成 非均相电解 二苯重氮甲烷 碘化合物 

分 类 号：TQ246.4[化学工程—有机化工]