反应详情

温度

120 °C

664 mg (3.36 mmol) of 6-chloro-4-nitro-1H-pyrrolo[2,3-b]pyridine, 1.39 g (10.1 mmol) of powdered potassium carbonate and 877 mg (5.04 mmol) of sodium dithionite are suspended in 10 ml of DMSO. The mixture is degassed, and 915 mg (5.04 mmol) of 4-amino-2,6-difluorophenol hydrochloride are added. The mixture is heated at 120° C. for 4 hours. After addition of ethyl acetate, the mixture is filtered off with suction through celite, and the celite is washed with ethyl acetate. The filtrate is shaken three times with saturated sodium bicarbonate solution and with saturated, sodium chloride solution. The filtrate is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by column chromatography (silica gel 60, mobile phase: dichloromethane/methanol=50:1).

1. customThe mixture is degassed
2. filtrationthe mixture is filtered off with suction through celite
3. washthe celite is washed with ethyl acetate
4. dry with materialThe filtrate is dried over sodium sulfate
5. customthe solvent is removed under reduced pressure
6. customThe residue is purified by column chromatography (silica gel 60, mobile phase: dichloromethane/methanol=50:1)