反应详情

温度

90 °C

To a stirred solution of methyl 3-(5,5-dimethylcyclopent-1-enyl)-4-(trifluoromethylsulfonyloxy)benzoate T3.5 (0.400 g, 1.1 mmol) in DMF (4.00 mL) at 23° C. was added 5-ethoxy-2-fluorophenylboronic acid (0.29 g, 1.6 mmol, commercially available from Sigma-Aldrich, St. Louis, Mo., USA), potassium carbonate (0.44 g, 3.2 mmol), and then tetrakis(triphenylphosphine)palladium (0.12 g, 0.11 mmol). The mixture was heated to 90° C. and stirred for 21 hours. The mixture was then cooled to room temperature, 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 (0-10% EtOAc in hexanes) to yield T25.1 as a colorless oil (0.350 g, 90% yield).

1. temperatureThe mixture was then cooled 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 (0-10% EtOAc in hexanes)