反应详情

温度

140 °C

Into a reaction flask, methyl isocyanate (6.5 mg, 0.11 mmol) is combined with N-{2,4-difluoro-3-[5-(1H-indazol-5-yl)-1H-pyrrolo[2,3-b]pyridine-3-carbonyl]-phenyl}-2,5-difluoro-benzenesulfonamide (P-0002, 22 mg, 0.031 mmol), tetrakis(triphenylphosphine)palladium(0) (2.2 mg, 0.0019 mmol), potassium carbonate (1.0 mL, 1.0 M in water) and 3 mL of acetonitrile. The reaction is heated at 140° C. for 50 minutes in a microwave, then diluted with water and ethyl acetate. The organic layer is washed with saturated sodium bicarbonate, then brine and dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is purified by silica gel column chromatography, eluting with methanol and dichloromethane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound (P-0003, 14 mg, 72%). MS (ESI) [M+H+]+=623.

1. washThe organic layer is washed with saturated sodium bicarbonate
2. dry with materialbrine and dried over sodium sulfate
3. filtrationfiltered
4. concentrationthe filtrate concentrated under vacuum
5. customThe resulting material is purified by silica gel column chromatography
6. washeluting with methanol and dichloromethane
7. concentrationconcentrated under vacuum