Hydroxyamine hydrochloride → HCID 86738350, compound

Participants

Reaction Steps

A solution of 13.66 g (40.37 mmol) of 7-acetyl-5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-2H-1,4-benzodiazepin-2-one and 13.6 g (0.196 mol) of hydroxylamine hydrochloride in 50 ml of pyridine is stirred at room temperature for 18 hours, then poured on to ice and extracted with methylene chloride/ethanol (9:1). The organic phase is washed successively with 3 N hydrochloric acid and water, dried and evaporated. The residue is chromatographed on 150 g of silica gel using methylene chloride as the elution agent and there is obtained, from ether, 5-(o-fluorophenyl)-1,3-dihydro-7-[1-(hydroxyimino)-ethyl]-1,3,3-trimethyl-2H-1,4-benzodiazepin-2-one of melting point 199°.

Provenance & Evidence