1, 3-Dienic δ-sultones 4, 6-diaryl-[1, 2] oxathiine 2, 2-dioxides were synthesized via a one- step reaction of arylalkynes with dioxane sulfotrioxide. The reactivity of various alkynes in this reaction was investigated. The resulting sultones were brominated with Br2 or N- bromosuccinimide regioselectively α to sulfur and subsequently coupled with phenylacetylene using Sonogashira conditions.