The enantioselective hydrolysis of -acetyloxymethyl--valerolactone was studied with various lipases. Among all of the lipases which were evaluated, PPL (porcine pancreatic lipase) in a phosphate buffer yielded the hydrolytic product (S)--hydroxymethyl--valerolactone and the unreacted substrate (R)--acetyloxymethyl--valerolactone with the highest optical purities.