The preparative electrosynthetic procedure for gram-scale preparation of symmetric 4,4′-dihydroxy-3,3′-diformylbiphenyls from salicylic aldehydes via the intermediate formation of ethylene-bridged bis((2-hydroxybenzylidene)imino)nickel (II) complexes is reported for the first time. This procedure represents a practical route to the variety of rare bisphenol derivatives. The electrochemical aryl-aryl coupling via an oxidative CH – activation in NiSalens is exploited for facile and selective C−C bond formation.