反应详情

5-Chloro-1H-pyrrolo[2,3-b]pyridine (532, 0.068 g, 0.44 mmol) was combined with methanol (10 mL) and potassium hydroxide (0.16 g, 2.8 mmol). The mixture was stirred for 50 minutes, then 2-ethyl-5-(4-fluoro-benzylamino)-2H-pyrazole-3-carbaldehyde (530, 0.100 g, 0.40 mmol, prepared as described in Example 47, Scheme 162, Step 5) was added and the reaction was stirred overnight at room temperature and then concentrated. Ethyl acetate was added and the mixture was washed with sodium bicarbonate saturated solution and brine. After drying over anhydrous sodium sulfate the solvent was removed under reduced pressure. Purification with silica gel column chromatography eluting with a gradient of ethyl acetate (10-100%) in hexanes provided the desired compound (0.0033 g, 2%). MS (ESI) [M+H+]+=398.1.

1. stirringthe reaction was stirred overnight at room temperature
2. concentrationconcentrated
3. additionEthyl acetate was added
4. washthe mixture was washed with sodium bicarbonate saturated solution and brine
5. dry with materialAfter drying over anhydrous sodium sulfate the solvent
6. customwas removed under reduced pressure
7. customPurification with silica gel column chromatography
8. washeluting with a gradient of ethyl acetate (10-100%) in hexanes