extracting agent destroys the azeotrope composed of water and benzyl alcohol to bring benzyl acetate and benzyl alcohol to the column bottom the concentration of the acetic acid should be controlled to be not less than 10 mol based on the water at the acetic acid concentration of lower than 10 mol relative to water azeotropes composed of water and benzyl acetate and of water and benzyl alcohol are formed in the acetic acid water recovery column 10 thereby benzyl acetate and benzyl alcohol being distilled out from the column top which may make the intended separation impossible with the aforementioned material composition no problem is caused in the operation of the column however when the reaction is conducted at a higher concentration of water or at a lower hydrolysis conversion ratio the acetic acid concentration at the inlet of the acetic acid water recovery column becomes lower so that acetic acid should be replenished to increase the acetic acid concentration up to 10 mol relative to water the benzyl alcohol and benzyl acetate discharged from the bottom of the acetic acid water recovery column 10 is introduced to an alcohol concentration column 11 to obtain an azeotropic mixture composed of benzyl alcohol and benzyl acetate from the column top and benzyl acetate from the column bottom the benzyl acetate obtained from the column bottom is recycled to the hydrolysis reactor 9 since the bottom liquid contains a small amount of high boiling impurities including dibenzyl ether a part of the.