Electrochemical coupling of phenyl halide catalyzed by NiCl2bpy in DMF has been investigated in this paper. Stainless steel was used as cathode and zinc as anode. Effects of potential, temperature and catalyst on electrolyses were studied to optimize the electrolytic conditions, with the maximal isolated yield under potentiostatic electrolysis to be 85%. Cyclic voltammetry of NiCl2bpy in the presence of phenyl bromide has been studied and mechanisms, concerned with several kinds of nickel complex, have been summarized.
A novel electrochemical procedure for the synthesis of ethyl carbanilate from aniline and carbon dioxide was developed via the selective cathodic reduction of carbon dioxide in CO2-saturated DMF solution containing 0. 1 mol/L TEABr at room temperature, followed by the addition of Eft as an alkylating agent. The synthesis was carried outun der mild[p(CO2) = 1.0×10^5 Pa, t =20 ℃ ] and safe conditions. Influences of the nature of the electrodes, the current densities, the passed charges during electrolysis, temperatures, and supporting electrolytes on the yield of ethyl carbanilate were studied to optimize the electrolytic conditions. The selectivity of ethyl carbanilate is 100%.
NIU Dong-fang XU Cheng-tian LUO Yi-wen ZHANG Li LU Jia-xing