The three isomeric symmetrical dimethylazoxybenzenes have been prepared in very good yield by oxidation of the corresponding azobenzenes with peracetic acid. 2,2′- and 4,4′-Diethylazoxybenzenes have been synthesized by oxidation of the azobenzenes and reduction of the ethylnitrobenzenes. The diethylazoxybenzenes were also reduced to the corresponding azo-and hydrazo-benzene derivatives.