反应详情

Into a reaction flask under nitrogen, [3-(5-bromo-1H-pyrrolo[2,3-b]pyridine-3-carbonyl)-2,4-difluoro-phenyl]-carbamic acid methyl ester (6, 15.00 g, 36.6 mmol) is combined with 300 mL of anhydrous acetonitrile and trimethylsilyl iodide (21.95 g, 109.7 mmol). The reaction is stirred at room temperature overnight, then diluted with 500 mL of ethyl acetate and washed with 2×500 mL of 10% aqueous sodium thiosulfate. The aqueous layers are combined and back extracted with 1×500 mL of ethyl acetate. The organic layers are combined and washed with 1×500 mL of saturated aqueous sodium bicarbonate, dried over magnesium sulfate, filtered and the filtrate concentrated under vacuum to provide the desired compound (7, 13.34 g).

1. washwashed with 2×500 mL of 10% aqueous sodium thiosulfate
2. extractionback extracted with 1×500 mL of ethyl acetate
3. washwashed with 1×500 mL of saturated aqueous sodium bicarbonate
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationthe filtrate concentrated under vacuum