Lipase-catalyzed acylation of racemic alcohols with a highly fluorinated acyl donor allows theirkinetic resolution accompanied by the simultaneous enantiomer-selective fluorous phase labeling.Both the tagged and the untagged enantiomer can be separated without chromatography by a veryefficient partition between a fluorous and an organic phase. The method has been successfullyapplied to the resolution of typically racemic secondary alcohols of low molecular weight. Thefluorous label can be recovered quantitatively.