Bromine → HCID 19760189, compound

Participants

Reaction Steps

A solution of 18.0 g of 2,3,4,5-tetrahydro-1,3,3-trimethyl-2-oxo-1H-1-benzazepine in 250 ml of methylene chloride was treated with 2.0 g of iron powder and thereafter dropwise with 5.83 ml of bromine in 30 ml of methylene chloride. The reaction mixture was heated to reflux overnight, thereafter poured on to ice, extracted with diethyl ether, washed with sodium pyro- sulphite solution, water and saturated sodium chloride solution, dried and evaporated. Crystallization from ethyl acetate/n-hexane yielded 21.4 g of pure 7-bromo-2,3,4,5-tetrahydro-1,3,3-trimethyl-2-oxo-1H-1-benzazepine.

Provenance & Evidence