A heat-gun dried 100-mL two-neck round bottom flask was charged with a stir bar and 1,1dibromo-2,2-bis(chloromethyl)cyclopropane (5.94 g, 10 mmol, 1.0 equiv.). The flask was evacuated and backfilled with N2. Next, 20 mL of anhydrous Et2O was added via syringe. The solution was cooled to -45 °C. Phenyllithium (PhLi) (1.8 M in n-Bu2O, 22 mL, 40 mmol, 2.0 equiv.) was added dropwise. Upon addition of PhLi, the reaction mixture turned brown, and a precipitate formed. The reaction was allowed to stir at -45 °C for 20 min and was then transferred to an ice bath and stirred at 0 °C for 2 h. After 2 h, a short path condenser connected to a 100 mL 2-neck receiver flask was introduced. The system was placed under vacuum for 2 min, then static vacuum was maintained. (Care should be taken not to pull the crude solution over through the distillation head -vigorous bubbling was observed) Vacuum may be reapplied periodically to increase the rate of the distillation. After the distillation is complete, the resulting solution of [1.1.1]propellane was transferred via cannula to a Teflon-capped 25 mL Schlenk tube. (It should be noted that the solution of propellane could be stored over 3 Å molecular sieves in a -20 °C freezer for multiple weeks without noticeable decomposition).