A process for producing 4,6-bis(substituted)phenyl-azoresorcinol of formula 2! ##STR6## wherein R represents halogen atom, C.sub.1-5 alkyl group, hydroxycarbonyl group or C.sub.1-5 alkoxy group, n represents 0 or an integer of 1 to 5, and two or more Rs may be the same or different from each other, which comprises reacting, in an alkaline solvent, resorcinol with a (substituted)benzenediazonium salt of formula 1! ##STR7## wherein R and n are the same as defined in the above formula 1!, and X represents Cl, Br, OSO.sub.3 H or OPO.sub.3 H.sub.2, characterized in that
- (a) a solution of the (substituted)benzenediazonium salt of formula 1! is mixed with a solution or suspension of an alkali metal or alkaline earth metal hydroxide to obtain an alkaline mixture, and this alkaline mixture is then mixed to be reacted with a solution or suspension containing resorcinol and/or its alkali metal salt or alkaline earth metal salt, or
- (b) a resorcinol is reacted with the (substituted)benzenediazonium salt in the presence of an alkali metal hydroxide or alkaline earth metal hydroxide 15 to 40 times by mol as much as the resorcinol.