Enantiomerically enriched phenylalanine-and leucine aldehyde analogues have been prepared by lipase catalyzed desymmetrization or kinetic resolution of 1, 3-propanediol derivatives as key steps. Observations of unusual enantioselectivity were made, and most notably, Candida antarctica lipase B showed an opposite enantiopreference from other lipases, which was exploited in the synthesis. A thorough evaluation of chemoenzymatic ...