γ-Thiolactones [5-alkyldihydro-2 (3 H)-thiophenones] and δ-thiolactones (6-alkyltetrahydro-2 H-thiopyran-2-ones) were synthesized via isothiouronium salts by reaction of the corresponding oxygen-containing lactones with thiourea and hydrobromic acid. The identity of the compounds was confirmed by means of IR, MS, and 1H and 13C NMR. Separation of the enantiomers of the thiolactones was achieved by capillary GC using heptakis (2, 3-di- ...