反应详情

To a room temperature solution of 2,6-dimethyl-3-pyridinol (3 g, 24.35 mmol) in THF (30 ml) was added cesium carbonate (15.87 g, 48.71 mmol) and 3,4-difluoro-1-nitro-benzene (3.87 g, 24.35 mmol). The reaction mixture was heated at reflux for 2 hours. After cooling to room temperature the solids were filtered off and the filtrate was evaporated till dryness. The crude product was purified by column chromatography (silica gel; DCM to DCM/MeOH(NH3) up to 2% as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate 9 (5.88 g, 92%).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 2 hours
3. filtrationwere filtered off
4. customthe filtrate was evaporated till dryness
5. customThe crude product was purified by column chromatography (silica gel; DCM to DCM/MeOH(NH3) up to 2% as eluent)
6. customThe desired fractions were collected
7. customevaporated in vacuo