反应详情

A mixture of the title compound of Example 78 (200 mg, 0.42 mmol),and copper (II) sulphate pentahydrate (150 mg, 0.60 mmol) in 2-methoxyethylamine (2 ml) was heated under reflux for 2 hours, then cooled. The reaction was partitioned between dichloromethane (20 ml) and aqueous sodium carbonate solution (5 ml), and the layers separated. The organic phase was dried (Na2SO4) and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel using an elution gradient of dichloromethane: methanol (98:2 to 95:5) to afford the title compound (150 mg, 69%).

1. temperaturewas heated
2. temperatureunder reflux for 2 hours
3. temperaturecooled
4. customThe reaction was partitioned between dichloromethane (20 ml) and aqueous sodium carbonate solution (5 ml)
5. customthe layers separated
6. dry with materialThe organic phase was dried (Na2SO4)
7. customevaporated under reduced pressure
8. customThe residue was purified by column chromatography on silica gel using an elution gradient of dichloromethane: methanol (98:2 to 95:5)