Hydroxyamine hydrochloride → HCID 178463012, compound

Participants

Reaction Steps

Intermediate 137 (3.50 g, 12.9 mmol), hydroxylamine hydrochloride (3.30 g, 47.8 mmol) and sodium hydrogencarbonate (4.01 g, 47.8 mmol) in EtOH (45 ml) were heated at 45° C. for 1.5 hours then at 50° C. for 2.5 hours. The suspension was concentrated in vacuo and the solid stirred in dichloromethane (80 ml) for 0.5 hours. The mixture was filtered and the solid stirred in EtOH, the resultant mixture was filtered and the filtrate evaporated. The solid was then washed with dichloromethane three time to afford Intermediate 138 as a white solid (1.62 g). LCMS showed MH+=305; TRET=1.85 min

Provenance & Evidence