标题:
2-氨基-5-溴-N,3-二甲基苯甲酰胺的电化学合成Electrochemical Synthesis of 2-Amino-5-Bromo-N,3-Dimethylbenzamide
作者:
杨雷, 王波, 郑瀚骁, 刘波, 由君, 吴绵园
关键字:
电化学, 2-氨基-N, 3-二甲基苯甲酰胺, 2-氨基-5-溴-N, 3-二甲基苯甲酰胺Electrochemical, 2-Amino-N, 3-Dimethylbenzamide, 2-Amino-5-Bromo-N, 3-Dimethylbenzamide
期刊名称:
《Journal of Organic Chemistry Research》, Vol.2 No.2, 2014-06-17
摘要:
在单室电解池中，金属铂片为阴阳电极，稀硫酸为支持电解质，40%氢溴酸为反应物，THF为溶剂，室温，2-氨基-N,3-二甲基苯甲酰胺在1.3~2.0 V电压下恒电流电解可以高产率地合成2-氨基-5-溴-N,3-二甲基苯甲酰胺。经反应条件优化，2-氨基-N,3-二甲基苯甲酰胺电化学溴化的最佳条件为：支持电解质为H2SO4，浓度为10%、40%HBr用量为8.0 mL，电流密度0.4 A，在此条件下反应电压为1.32~1.65 V，溴化产物收率为97.3%，电流效率为88.3%。
In a single-chamber electrolytic cell, platinum as the anode and cathode, dilute sulfuric acid as the supporting electrolyte, 40wt.% hydrobromic acid in H2O as the reactant, 2-amino-N,3-dimethylbe- nzamide can be highly synthesized into 2-amino-5-bromo-N,3-dimethylbenzamide by the constant- current electrolysis under the voltage from 1.3 V to 2.0 V at room temperature. The optimum of reaction conditions is as follows: electrolyte is H2SO4, the volume of hydrogen bromide is 8 mL, current density is 0.4 A, the reaction voltage is 1.32 - 1.65 V, product yield is 97.3% and the current efficiency was 88.3%.