反应详情

温度

25 °C

To a 250 mL round bottomed flask charged with 1-(1-benzenesulfonyl-5-methoxy-1H-pyrrolo[2,3-b]pyridin-2-yl)-2-(tetrahydro-furan-2-yl)-ethanol (2.5 g, 6.2 mmol) in dichloromethane (200 mL) was added Dess-Martin periodinane (6.6 g, 15.5 mmol) at 25° C. The reaction mixture was stirred at 25° C. for 1 h and then quenched with a saturated aqueous sodium bicarbonate solution (60 mL). The mixture was extracted with ethyl acetate (250 mL), washed with a saturated aqueous sodium bicarbonate solution (3×50 mL), brine, dried over anhydrous sodium sulfate and then concentrated in vacuo to give 1-(1-benzenesulfonyl-5-methoxy-1H-pyrrolo[2,3-b]pyridin-2-yl)-2-(tetrahydro-furan-2-yl)-ethanone (1.7 g, 71%) as a light yellow solid which was used in the next step without further purification: LC/MS m/e calcd for C20H20N2O5S [M+H]+ 401.46, observed 401.2.

1. customquenched with a saturated aqueous sodium bicarbonate solution (60 mL)
2. extractionThe mixture was extracted with ethyl acetate (250 mL)
3. washwashed with a saturated aqueous sodium bicarbonate solution (3×50 mL), brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo