PURPOSE: To easily obtain the subject compound in high purity by reacting a specific compound with an ester in the presence of an enzyme and absence of water to effect ester interchange reaction.

CONSTITUTION: A substrate (C) is produced by compounding (A) a racemic compound of formula I (n is 0 or 1; one of R1 and R2 is OH; when R1 is OH, R2=R3=H or R2=R3=CH3 ; when R2 is OH, R1=R3=M) with (B) an ester such as vinyl acetate at a molar ratio of 1 to 0.5-2. An enzyme such as lipase is added to the component C and subjected to asymmetric ester interchange reaction in the absence of solvent at 15-45°C for 5-240hr. The objective optically active hydroxylactone can be produced by filtering and purifying the obtained reaction product (D) by column chromatography and resolving the product into esters of an optically active alcohol of formula II (* represents asymmetric C when bonded with hydroxy group) rich in either R-isomer or S-isomer and its antipode.