A process for preparing a metal phenolate of the formula II:Cl--Ar.sub.1 COAr.sub.2 OM (II)wherein each of Ar.sub.1 and Ar.sub.2 which may be the same or different is a bivalent group of the formula: ##STR1## wherein each of R.sup.1 and R.sup.12 is a hydrogen atom, a halogen atom, an alkoxy group, a phenoxy group, an alkyl group, a cycloalkyl group, a phenyl group, an aralkyl group, an acyl group, a nitrile group, a nitro group or an acyloxy group, each of Y and Z is an oxygen atom or a ketone group, and each of n and m is an integer of from 0 to 4, and M is an alkali metal, which comprises reacting a phenol compound of the formula I:Cl--Ar.sub.1 COAr.sub.2 OH (I)wherein Ar.sub.1 and Ar.sub.2 are as defined above, with an alkali metal compound in the presence of water, and then removing water, characterized in that water is azeotropically distilled off together with an organic solvent capable of forming an azeotropic mixture with water.