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.