To provide a method for the single-stage production of stable 3,3'-bis(trifluoromethyl)hydrazobenzene usable as a raw material for 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl which is useful as a raw material for polyimide by using m-nitrobenzotrifluoride as a starting raw material.

3,3'-Bis(trifluoromethyl)hydrazobenzene is produced by reducing m-nitrobenzotrifluoride with zinc in the presence of an organic solvent and an alkaline aqueous solution to obtain 3,3'-bis(trifluoromethyl)hydrazobenzene and adjusting the pH of the reaction liquid to 6-11 after completing the reduction reaction.