反应详情

温度

100 °C

To a solution of 1-(benzyl)-4-(bromo)-5-(2,4-difluorophenyl)-2-(methyl)-imidazole (1.12 g, 3.08 mmol) in 8 mL DME, add 1-isopropylsulfonyl-2-amino-benzimidazole-6-boronic acid (2.62 g, 9.25 mmol). Add sodium carbonate (0.98 g, 9.25 mmol) dissolved in 1 mL of water and trans-dichlorobis(triphenylphosphine) palladium (II) (0.65 g, 0.93 mmol). Heat the mixture to 100° C. with stirring under nitrogen. After 3 hours, cool the solution and filter over a pad of Celite® and sodium sulfate. Purify the residue by radial chromatography eluting with 3% methanol in CH2Cl2 with a gradient to 10% methanol. Perform a second purification by radial chromatography eluting with 4% methanol in CH2Cl2 with a gradient to 6% methanol to yield 390 mg (24%) of the title compound as a yellow solid. MS(ES+): m/z=522.0 (M+H)+

1. temperaturecool the solution
2. filtrationfilter over a pad of Celite® and sodium sulfate
3. customPurify the residue by radial chromatography
4. washeluting with 3% methanol in CH2Cl2 with a gradient to 10% methanol
5. customa second purification by radial chromatography
6. washeluting with 4% methanol in CH2Cl2 with a gradient to 6% methanol