PURPOSE: To recover an organic solvent under a mild condition by a simple operation after production of chloranil and to reuse the recovered organic solvent for production of chloranil.

CONSTITUTION: Hydroquinone is reacted with chlorine in a heterogeneous mixed solvent of water or hydrochloric acid and an organic solvent such as o- dichlorobenzene non-compatible with the water or hydrochloric acid to produce chloranil. Chloranil is separated from the organic solvent non-compatible with water or hydrochloric acid and chlorine dissolved in the organic solvent incompatible with water or hydrochloric acid and ≥2 mols based on hydrochloric acid of an aqueous solution of an alkali such as an aqueous solution of sodium hydroxide are brought into contact with the organic solvent incompatib1e with water or hydrochloric acid.