Phosphorus pentachloride → HCID 67812971, compound

Participants

Reaction Steps

To a round bottomed flask was added 1-methyl-4-(trifluoromethyl)-4H-benzo[c]isoxazolo[4,5-e]azepin-6(5H)-one (86 mg, 0.305 mmol), DCM (2 mL), and PCl5 (102 mg, 0.488 mmol). The solution was stirred at room temperature for 30 min before addition of more PCl5 (˜0.5 eq). The solution was stirred at room temperature for 4 h before pouring onto an ice-saturated aqueous NaHCO3 mixture. The layers were separated and the aqueous phase was extracted with DCM. The combined organic phase was dried over Na2SO4, filtered, and concentrated. The crude residue was purified via Biotage (EtOAc/hex) to afford the titled compound (52.9 mg, 0.176 mmol). LC/MS m/z 301 [M+H]+.

Provenance & Evidence