反应详情

温度

25 °C

To a solution of 1-(1-benzenesulfonyl-1H-pyrrolo[2,3-b]pyridin-2-yl)-3,3-dimethyl-butan-1-ol (3.1 g, 8.7 mmol) in dichloromethane (150 mL) was added Dess-Martin periodinane (9.3 g, 22 mmol) at 25° C. The reaction mixture was stirred at 25° C. for 2 h and then quenched with a saturated aqueous sodium bicarbonate solution (100 mL). The mixture was extracted with dichloromethane (50 mL), washed with a saturated aqueous sodium bicarbonate solution (3×100 mL), brine, dried over anhydrous sodium sulfate and then concentrated in vacuo to afford 1-(1-benzenesulfonyl-1H-pyrrolo[2,3-b]pyridin-2-yl)-3,3-dimethyl-butan-1-one (2.5 g, 83%) as a light yellow solid which was used in the next step without further purification: LC/MS m/e calcd for C19H20N2O3S [M+H]+ 357.45, observed 357.3.

1. customquenched with a saturated aqueous sodium bicarbonate solution (100 mL)
2. extractionThe mixture was extracted with dichloromethane (50 mL)
3. washwashed with a saturated aqueous sodium bicarbonate solution (3×100 mL), brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo