An oven-dried microwave vial equipped with a stir bar was introduced to the glovebox, and the (chlorotetrafluoro-λ 6 -sulfanyl)arene was added (0.1 mmol. 1.0 equiv.); the vial was sealed with a crimper. The reaction vessel was removed from the glovebox, wrapped in aluminum foil, and anhydrous Et2O (0.76 mL) was added. The solution was cooled to -45 °C in an acetonitrile dry ice bath; a solution of [1.1.1]propellane (0.5 M in Et2O, 0.24 mL, 1.2 equiv.) was added in one portion down the side of the reaction vessel. The reaction was then transferred to an ice bath and stirred for 3 h at 0 °C. The crude reaction mixture was then concentrated in vacuo. The final product was isolated by column chromatography with hexanes and ethyl acetate. (Solvent systems for individual compounds are given below). Note: the concentration of the [1.1.1]propellane solution was variable between batches; the necessary volume of this solution was calculated and Et2O was added to give a concentration of 0.1 M with respect to the limiting reagent.