反应详情

To a solution of 4-amino-2-fluorophenol (254 mg, 2.0 mmol) in DMF (5 mL) was added t-BuOK (359 mg, 3.2 mmol). The mixture was stirred at rt for 30 minutes. 3,4-dichloropicolinamide (420 mg, 2.2 mmol) was then added, and the mixture was microwaved at 120° C. for 2 hours. The mixture was cooled to rt, quenched with 25 mL of water. The resulted solution was extracted with EtOAc (30 mL×3) and the combined organic phases were washed with brine (30 mL×3), dried over Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (EtOAc/PE (v/v)=2/1) to give the title compound as a pale yellow solid (306 mg, 54.4%).

1. customthe mixture was microwaved at 120° C. for 2 hours
2. temperatureThe mixture was cooled to rt
3. customquenched with 25 mL of water
4. extractionThe resulted solution was extracted with EtOAc (30 mL×3)
5. washthe combined organic phases were washed with brine (30 mL×3)
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. customThe residue was purified by a silica gel column chromatography (EtOAc/PE (v/v)=2/1)