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%。
Abstract:
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%.