Abstract: 2,2-Dimethoxy-2-phenylacetophenone is prepared by reacting benzil with dimethyl sulfate and alkali metal methylate in a nonpolar organic solvent (e.g. xylene, cyclohexane) in the presence of one or more of catalysts selected from the group consisting of polyethylene glycol, a polyethylene glycol dialkyl ether and a crown ether. The reaction can be carried out more preferably in the presence of diglyme or triglyme or a mixture of diglyme or triglyme and polyethylene glycol.