Optimum conditions for electrosynthesis of nitrosobenzenes bearing in meta or para position electron withdrawing groups (CN, COO-, COOMe, CHO, COMe) were found using de polarography, cyclic voltammetry, and the recording of. current-voltage curves using mercury and carbon electrodes. Electroreduction was best carried out in an acetate buffer pH 5.7 containing 20 to 40% dimethylformamide using a porous carbon electrode. This was followed by electro-oxidation on an anode of a similar composition in the same solution. Two consecutive batch electrolyses are possible, but yields with a flow-through cell were better due to a smaller effect of consecutive condensations, yielding azoxy or azomethine compounds. At pH 5.7, which was used in this study, the rates of these competitive processes were lowest.