反应详情

温度

0 °C

To a cold (0° C.) solution of 5-fluoro-4-methoxy-1-tosyl-1H-pyrrolo[2,3-b]pyridine, 68b, (0.79 g, 2.45 mmol) in chloroform (50 mL) was added bromine (0.13 mL, 2.45 mmol). The reaction mixture was stirred at 0° C. for 3 hours and then slowly warmed to ambient temperature. The mixture was diluted with deionized water and quenched with aqueous sodium bicarbonate. The aqueous phase was extracted with methylene chloride and dried over sodium sulfate. The resulting solid was purified via silica gel chromatography (15-30% EtOAc/Hexanes) to give 170 mg of the desired product.

1. temperatureslowly warmed to ambient temperature
2. customquenched with aqueous sodium bicarbonate
3. extractionThe aqueous phase was extracted with methylene chloride
4. dry with materialdried over sodium sulfate
5. customThe resulting solid was purified via silica gel chromatography (15-30% EtOAc/Hexanes)