Hydroxyamine hydrochloride → HCID 23333613, compound

Participants

Reaction Steps

Methyl 5,6-dihydro-5-methyl-11-oxodibenz[b,e]azepine-2-acetate (1.5 g) was dissolved in methanol (80 ml), and hydroxylamine hydrochloride (1.0 g) was added to make a homogeneous solution. Then, a 28% solution (6 g) of sodium methylate in methanol was added to the homogeneous solution, and the mixture was heated for 3 hours. Then, the reaction mixture was concentrated, and after addition of water (20 ml) and dry ice (1 g), was extracted with chloroform. The extract was dried over MgSO4, and then, chloroform was distilled off. The residue was stirred with benzene to form crystals. The crystals were recrystallized from benzene-tetrahydrofuran to obtain the desired compound (0.8 g) as yellow prismatic crystals.

Provenance & Evidence