Abstract: The reaction residue containing diaryl alkylphosphonate resulting from the reaction of triaryl phosphite and alcohol in the presence of a rearrangement catalyst is treated by optionally, and preferably, stripping phenol by-product therefrom, optionally, and then treating the residue with aqueous dilute acid to convert unreacted triaryl phosphite reagent to diaryl phosphite and remove it as an aqueous layer, and then treating the remaining residue with an aqueous base to yield a water phase containing the unwanted diarylphosphite by-product and an organic phase containing the desired diaryl alkylphosphonate, with subsequent removal of the water phase, prior to subsequent distillation of the remaining organic phase residue to remove purified diaryl alkylphosphonate therefrom.