The asymmetric resolution of various 1-aryl-3-buten-1-ols via microbial hydrolysis of the corresponding acetates has been investigated using different Rhizopus species. The chosen species, R. arrhizus ( wild type), efficiently hydrolyzed 1-phenyl- and 1-para-substituted phenyl-3-buten-1-ol acetates, producing the enantiomerically pure (R)-alcohols with 53 - 65% yields. Although the antipode acetates were obtained with 9 - 52% enantiomeric excess, the (S)- alcohols were amenable in > 99% enantiomeric excess via a R. arrhizus mediated asymmetric reduction of the corresponding ketones.