反应详情

温度

90 °C

To a stirred solution of 66.13B (1.00 g, 2.9 mmol) in DMF (12 mL) at 23° C. was added 5-fluoro-2-methoxypyridin-4-ylboronic acid (0.75 g, 4.4 mmol) (commercially available from Asymchem), potassium carbonate (1.2 g, 8.8 mmol), followed by tetrakis(triphenylphosphine)palladium (0.24 g, 0.20 mmol). The mixture was heated to 90° C. The reaction mixture was then stirred for 17 hours and then cooled to room temperature. The reaction was diluted with brine and extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and the product was then purified on silica gel (0-30% EtOAc in hexanes) to yield 83.21A as a colorless solid (0.860 g, 92% yield).

1. temperaturecooled to room temperature
2. extractionextracted three times with EtOAc
3. dry with materialAfter drying over anhydrous magnesium sulfate
4. filtrationfiltering
5. customthe organic solvent was removed under reduced pressure
6. customthe product was then purified on silica gel (0-30% EtOAc in hexanes)