A series of dihalogenated and five tetrachloroazobenzenes were oxidized to the corresponding azoxy compounds by means of 30% hydrogen peroxide in glacial acetic acid, the reaction being carried out at about 60–70 °C, for 24 hoursAs expected, the yields, in general, obtained from azobenzenes containing substituents in the 2,2′-positions were lower than those from compounds having substituents in the 3,3′- and 4,4′-positions, which gave very good results.