Methyl iodide → HCID 15168927, compound

Participants

Reaction Conditions

Reaction Steps

To a warm solution of 4.05 g potassium methoxide in 80 ml of t-butanol and 80 ml of dioxane was added 13.5 g (0.05 mol) of 2-nitro-7-methyldibenz[b,f][1,4]oxazepin-11(10H)-one. The resulting suspension was warmed to 60° C. for 15 minutes. Initially everthing went in solution, after several minutes a crystalline precipitate formed. To the stirred suspension was added 3.75 ml of iodomethane. The reaction mixture was stirred for 4 hours at 60° C., then concentrated to dryness in vacuo. The dark residue was suspended in water, acidified with acetic acid, concentrated in vacuo and then recrystallized from propanol to give 8.5 g (60% yield) of 2-nitro-7,10-dimethyldibenz[b,f][1,4]- oxazepin-11(10H)-one mp 156°-159°.

Provenance & Evidence