Optically active butenolide and gamma-butyrolactone derivatives were prepared by removing (R)-phenyl glycinol and (1R, 2R)-norpseudoephedrine used as chiral auxiliaries from butenolides and gamma-butyrolactones in two steps. The structures of these products were determined using H-1 NMR, C-13 NMR, Mass spect., IR and microanalysis.