反应详情

温度

120 °C

300 mg (1.16 mmol) of 1-acetyl-4,6-dichloro-3-methyl-1H-pyrrolo[2,3-b]pyridine (from example XL) and 320 mg (2.32 mmol) of powdered potassium carbonate are suspended in 9 ml of DMSO. The mixture is degassed, and 442 mg (3.48 mmol) of 4-amino-2-fluorophenol 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 (diatomaceous earth) and the filtercake is washed with ethyl acetate. The filtrate is extracted three times with sat. sodium bicarbonate solution and with sat. 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: DCM:methanol=50:1).

1. customThe mixture is degassed
2. filtrationthe mixture is filtered off with suction through CELITE (diatomaceous earth)
3. washthe filtercake is washed with ethyl acetate
4. extractionThe filtrate is extracted three times with sat. sodium bicarbonate solution
5. dry with materialThe filtrate is dried over sodium sulfate
6. customthe solvent is removed under reduced pressure
7. customThe residue is purified by column chromatography (silica gel 60, mobile phase: DCM:methanol=50:1)