反应详情

温度

160 °C

In a microwave vial, N-[3-(5-bromo-1H-pyrrolo[2,3-b]pyridine-3-carbonyl)-2-fluoro-phenyl]-2-fluoro-benzenesulfonamide (21, 100 mg, 0.203 mmol), 2-methoxy-5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyrimidine (22, 72 mg, 0.305 mmol) and tetrakis-(triphenylphosphine) palladium(0) (10 mg) are combined with potassium carbonate (0.609 mL, 1M aqueous, 0.609 mmol) and 0.6 mL of acetonitrile. The reaction mixture is heated in a microwave at 160° C. for 15 minutes. The mixture is filtered through celite, and the celite is washed with water and ethyl acetate. The aqueous layer is separated from the filtrate and extracted with ethyl acetate. The organic portions are combined and washed with brine, then 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-1518, 27 mg). MS (ESI) [M+H+]+=521.95.

1. filtrationThe mixture is filtered through celite
2. washthe celite is washed with water and ethyl acetate
3. customThe aqueous layer is separated from the filtrate
4. extractionextracted with ethyl acetate
5. washwashed with brine
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationthe filtrate concentrated under vacuum
9. customThe resulting material is purified by silica gel column chromatography
10. washeluting with methanol and dichloromethane
11. concentrationconcentrated under vacuum