Resolution of alkyn-3-ols has been achieved using a lipase from Candida rugosa to esterify the alcohols with trifluoroethyl butyrate in hexane to give the O-alcohols and the (R)-esters. Subsequent reacylation of the product alcohols and alcoholysis of the esters with I-butanol furnished the O-alcohols with good (86-91% ees) and the (R)-butyrate with moderate enantiomeric purities (62-64% ees).