The resolution of racemic citronellol and menthol by enzymatically catalyzed transesterification in supercritical carbon dioxide (SC-CO2) was investigated. Different lipases and an esterase in connection with various acylating reagents were employed. While the transesterification of (+/-)-menthol was reasonably fast and gave high enantiomeric excess, resolution of (+/-)-citronellol was not feasible.