反应详情

温度

95 °C

A vial was charged with 3-chloro-7-(2-fluoropyridin-3-yl)-5H-chromeno[2,3-c]pyridin-5-one (275 mg, 0.842 mmol), neopentyl alcohol (297 mg, 3.37 mmol), Pd2 dba3 (38.5 mg, 0.042 mmol), racemic-2-(di-t-butylphosphino)-1,1′-binaphthyl (67.1 mg, 0.168 mmol) and cesium carbonate (686 mg, 2.104 mmol). The vial was evacuated and backfilled with nitrogen (procedure was repeated twice). Toluene (1.7 mL) was added, the vial was sealed and the reaction mixture was heated to 95° C. in an oilbath overnight. The reaction mixture was cooled to RT and partitioned between EtOAc and water. The organic phase was separated and dried over MgSO4. The solvent was removed under reduced pressure and the residue was purified by flash chromatography (10-100% EtOAc/hexanes). 7-(2-Fluoropyridin-3-yl)-3-(neopentyloxy)-5H-chromeno[2,3-c]pyridin-5-one (60 mg) was obtained as a yellow powder.

1. customThe vial was evacuated
2. additionToluene (1.7 mL) was added
3. customthe vial was sealed
4. temperatureThe reaction mixture was cooled to RT
5. custompartitioned between EtOAc and water
6. customThe organic phase was separated
7. dry with materialdried over MgSO4
8. customThe solvent was removed under reduced pressure
9. customthe residue was purified by flash chromatography (10-100% EtOAc/hexanes)