反应详情

温度

160 °C

In a 10 mL microwave vial, propane-1-sulfonic acid [3-(5-bromo-1H-pyrrolo[2,3-b]pyridine-3-carbonyl)-2,4-difluoro-phenyl]-amide (9, 51.0 mg, 0.111 mmol) and 4-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyrazol-1-yl]-piperidine-1-carboxylic acid tert-butyl ester (34, 84.2 mg, 0.223 mmol) are combined with 0.680 mL of acetonitrile and potassium carbonate (0.34 mL, 1.00 M in water). 1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (8.3 mg, 0.011 mmol) is added and the mixture is heated at 160° C. in the microwave for 5 minutes, then diluted with water and extracted with ethyl acetate. The organic layer is washed with water, brine, and dried with magnesium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is purified by silica gel column chromatography, eluting with ethyl acetate and hexane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound (P-1001, 47 mg). MS (ESI) [M+H+]+=629.0.

1. extractionextracted with ethyl acetate
2. washThe organic layer is washed with water, brine
3. dry with materialdried with magnesium sulfate
4. filtrationfiltered
5. concentrationthe filtrate concentrated under vacuum
6. customThe resulting material is purified by silica gel column chromatography
7. washeluting with ethyl acetate and hexane
8. concentrationconcentrated under vacuum