Tetrahydrofuran → HCID 15981767, compound

Participants

Reaction Conditions

Reaction Steps

Trichlorobismuthane (1.25 g; 3.96 mmol) was dissolved in anhydrous THF (50 mL) and cooled to −10° C. Cyclopropylmagnesium bromide (0.5M in THF, 15 mmol; 30 mL) was added via dropping funnel over 30 min, keeping the temperature at −10° C. The reaction mixture was stirred at RT for 1 h then heated at 70° C. for 30 min, at which time a black precipitate was observed. After cooling to RT, the solution was cannulated under nitrogen over a degassed biphasic solution of brine (100 ml) and ether (100 ml). The heterogeneous solution was stirred for 5 min, transferred to a separatory funnel and diluted with ether (50 ml). The organic phase was collected, dried over sodium sulfate, filtered and concentrated under reduced pressure to give a yellow oily solid. Ether (25 ml) was added followed by hexane (25 ml). The mixture was sonicated, cooled to 0° C., and filtered to collect the light yellow solid, tricyclopropylbismuthane (770 mg, 58%).

Provenance & Evidence