Methylamine → HCID 22760079, compound

Participants

Reaction Steps

Crude 7-chloro-4-(2-chloroacetyl)-5-phenyl-2,3,4,5-tetrahydro-1,4-benzoxazepine, prepared as described in Example 4a starting with 7-chloro-5-phenyl-2,3,4,5-tetrahydro-1,4-benzoxazepine (1.82 g, 7.0 millimoles), was dissolved in 125 ml CH2Cl2 and the solution was saturated with gaseous monomethylamine. The reaction solution was stoppered and allowed to stand at room temperature for 18 hours, followed by unstoppering and warming on a steam bath for 30 minutes. The resulting CH2Cl2 solution was washed with two portions of saturated NaHCO3, dried over Na2SO4, filtered and rendered free of solvent to afford crude 7-chloro-4-(2-methylaminoacetyl)-5-phenyl-2,3,4,5-tetrahydro-1,4-benzoxazepine as a light viscous oil which was used directly in the next step without further purification.

Provenance & Evidence