Hydroxyamine hydrochloride → HCID 59003189, compound

Participants

Reaction Conditions

Reaction Steps

To a mixture of N-(3,5-Bis-trifluoromethyl-benzyl)-N-[8-chloro-1-(3-oxo-butyryl)-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl]-acetamide (0.13 mmol, 72 mg), hydroxylamine hydrochloride (1.3 mmol, 90 mg) in MeOH (2 mL) was added NaOAc (20 mg) at room temperature. The resulting suspension was stirred vigorously at 70° C. for 12 h. After completion, the mixture was diluted with water (20 mL), extracted with EtOAc (3×20 mL). The combined organic layers were washed with water and brine, dried over Na2SO4 and evaporated to dryness. Flash chromatography (EtOAc-Hexane as eluent 1:1) afforded the title compound as viscous foam; Rf 0.35 (EtOAc-Hexane, 1:1, v/v); MS (ES+): 564 (M+H2O).

Provenance & Evidence