反应详情

To a room temperature solution of 1-(4-fluorophenyl)-1H-pyrazolo[3,4-c]pyridine-4-carboxylic acid [(S)-1-(1H-pyrazol-3-yl)-propyl]-amide (0.040 g, 0.11 mmol) in THF was added 60% sodium hydride (9 mg, 0.2 mmol) in mineral oil. After 20 minutes, methansulfonyl chloride (25 mg, 0.22 mmol) was added. After 3 hours, the reaction was quenched with saturated aqueous ammonium chloride and the mixture was extracted with EtOAc. The combined organic layers were washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel chromatography (the column was equilibrated with dichloromethane-Et3N) eluting with 5% methanol in dichloromethane. Material from the column was crystallized in ether to afford the title compound.

1. waitAfter 3 hours
2. customthe reaction was quenched with saturated aqueous ammonium chloride
3. extractionthe mixture was extracted with EtOAc
4. washThe combined organic layers were washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was purified by silica gel chromatography (the column
8. washeluting with 5% methanol in dichloromethane
9. customMaterial from the column was crystallized in ether