反应详情

温度

90 °C

A mixture of 5-bromo-4-((2-chloropyridin-4-yl)oxy)-2-fluoroaniline (994 mg, 3.13 mmol), K3PO4 (1.993 g, 9.39 mmol) and 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (716 mg, 3.44 mmol) in DMF (10 mL) and water (1.5 mL) was sparged with Ar, treated with Pd(PPh3)4 (362 mg, 0.313 mmol) and heated at 90° C. overnight. The mixture was cooled to RT, diluted with water, extracted with EtOAc (2×) and the combined organics were washed with brine, dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (EtOAc/Hex) to afford 5-bromo-2-fluoro-4-((2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yl)oxy)aniline (594 mg, 52%). MS (ESI) m/z: (M+H+): 363.0.

1. customwas sparged with Ar
2. temperatureThe mixture was cooled to RT
3. extractionextracted with EtOAc (2×)
4. washthe combined organics were washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated to dryness
7. custompurified via silica gel chromatography (EtOAc/Hex)