反应详情

To a solution of crude ethyl 3-(3-hexyl-6-methyl-2-oxo-3-azabicyclo[3.1.0]hex-6-yl)benzenecarboximidoate (Preparation 42, 700 mg, 1.86 mmol) in methanol (5 ml) was added formic acid hydrazide (123 mg, 2.05 mmol) and the mixture was heated under reflux for 90 min. After cooling to room temperature, the solvent was removed in vacuo and the residue was heated to 150° C. for 12 h. The mixture was cooled and purified directly by silica column chromatography eluting with ethyl acetate:methanol (95:5) to afford the title compound (400 mg, 64%) as a colourless gum.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 90 min
3. customthe solvent was removed in vacuo
4. temperaturethe residue was heated to 150° C. for 12 h
5. temperatureThe mixture was cooled
6. custompurified directly by silica column chromatography
7. washeluting with ethyl acetate:methanol (95:5)