Bromotris(dimethylamino)phosphonium Hexafluorophosphate

Experimental procedure²⁾: A solution of 1 (80 mg, 0.189 mmol, 1.0 eq.) in acetonitrile (1.5 mL) and diethylamine (1.5 mL) is stirred at room temperature under N₂ for 30 min and then concentrated. The residue is concentrated twice more from acetonitrile and then suspended in CH₂Cl₂ (3 mL) under N₂. To this is added 2 (77 mg, 0.199 mmol, 1.15 eq.), DIPA (82 μL, 0.473 mmol, 2.5 eq.), and BroP (77 mg, 0.199 mmol, 1.05 eq.). The flask is flushed with N₂, stoppered, and left to stir at room temperature overnight. The mixture is concentrated and the residue applied to a flash column in a minimum volume of CH₂Cl₂. The column is eluted with 3:1 EtOAc - hexanes to afford 3 (106 mg, 98% yield).