A simple and effective oxidative dehydrogenation of nitro derivatives of bibenzyl was developed using a mixture of 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO) and metal salts as catalyst under an atmospheric pressure of oxygen. The oxidation of several nitro derivatives of bibenzyl led to corresponding nitro stilbene in good yields, and the yields increased with the increase in the substituted nitro group on the bibenzyl. For example, the aerobic dehydrogenation of 2,2’,4,4’,6,6’-hexanitrobibenzyl in the presence of a catalytic amount of TEMPO with metal salts gave 2,2’,4,4’,6,6’-hexanitrostilbene in 81% yield and 4,4’-dinitrostilbene-2,2’-disulfonic acid (75%) was obtained from 4,4’-dinitrobibenzyl-2,2’-disulfonic acid.