(R)-2-Chloro-l-(m-chlorophenyl)ethanol,a precursor of(R)-3-chlorostyrene oxide which is the key chiral intermediate for the preparation of severalβ3-adrenergic receptor agonists was prepared in 40%yield and 99%ee by the Lipozyme TL IM-catalyzed second resolution of the corresponding racemate in the presence of vinyl acetate. (R) -2-Chloro-l- (m-chlorophenyl) ethanol, a precursor of (R) -3-chlorostyrene oxide which is the key chiral intermediate for the preparation of several β3-adrenergic receptor agonists was prepared in 40% yield and 99% ee by the Lipozyme TL IM-catalyzed second resolution of the corresponding racemate in the presence of vinyl acetate.