Hydroxyamine hydrochloride → HCID 86738976, compound

Participants

Reaction Steps

A solution of 2-methoxy-5-methylene-10-oxo-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (9.7 g, 0.0388 mol), hydroxylamine hydrochloride (3.42 g, 0.0492 mol), and sodium acetate (4.26 g, 0.0519 mol) in methanol (194 ml) is heated under reflux for 2 hours. The solvent is removed under reduced pressure, the residue is slurried in water (200 ml), the pH is adjusted to 8 with concentrated aqueous ammonia, and the slurry is extracted with ether (3×105 ml). The combined extracts are dried over MgSO4 and filtered, and the filtrate is evaporated to yield 10.1 g (98%) of crude material. A sample recrystallized from ether has m.p. 125°-127° C.

Provenance & Evidence