Methanesulfonyl chloride → HCID 19872045, compound

Participants

Reaction Steps

Methanesulphonyl chloride (0.18 ml) was added dropwise to a solution of 7-amino-3-[2-(4-amino-3-methylphenoxy)ethyl]-1,2,4,5-tetrahydro-3H-3-benzazepine (0.36 g) in pyridine (30 ml) cooled to 0°, and the mixture was then stirred at room temperature for 72 hours. The solvent was evaporated in vacuo and the residue was taken up in methylene chloride and washed three times with saturated aqueous sodium bicarbonate and three times with brine. The organic layer was dried (Na2SO4), filtered and evaporated in vacuo to give an oil which was triturated with methylene chloride to give a solid. Recrystallisation of the solid from ethanol/ethyl acetate gave the title compound, yield 0.28 g, m.p. 173°-174°.

Provenance & Evidence