The present invention provides methods comprising distilling a reaction mixture of methacrolein and methanol used to make methyl methacrylate (MMA) in the presence of one or more strong or inorganic acids, the mixture comprising an aqueous organic component mixture of all of water, MMA, methacrolein methanol and acetals or hemiacetals of methacrolein to remove the acetals or hemiacetals of methacrolein to a level of 100 ppm or below, based on the amount of methyl methacrylate. The method reduces the amount of acetals or hemiacetals of methacrolein to well below equilibrium levels and eliminates the need for additional downstream distillation to refine the product of the reaction.