Hydroxyamine hydrochloride → HCID 86616068, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 8-Chloro-5-oxo-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid isopropyl ester (3.40 g, 12.1 mmole) in EtOH/H2O (96.0 ml/24.0 ml) was added hydroxylamine hydrochloride (8.39 g, 121 mmole) followed by sodium acetate (9.93 g, 121 mmole). The reaction was heated under 60° C. for 3 hours. The mixture was partitioned between ethyl acetate (100 ml) and 1.00N HCl (100 ml). After separated the two layers, the aqueous layer was extracted with more acetate (2×100 ml). The combined organics washed with NaHCO3 (aq) and followed by brine (2×200 ml). Dried over Na2SO4, filtered and concentrated to provide the crude product (3.45 g, 96%), which was used directly for the next step without further purification. MS (ES+): 297 (M+H).

Provenance & Evidence