反应详情

Combine 5-bromo-3-(2,2-dimethyl-propyl)-3H-imidazo[4,5-b]pyridin-2-ylamine (30.00 g, 105.94 mmol), Et3N (60 mL), and Pd(OAc)2[P(Ph)3]2 (3.97 g, 5.30 mmol) in toluene (150 mL) and heat the resulting mixture to ˜65° C. under nitrogen. Add 1-ethynyl-2,4-difluoro-benzene (21.95 g, 158.92 mmol) in toluene (30 mL) dropwise to the above mixture, and then heat the resulting reaction mixture at 80° C. for 3 h. Cool the reaction to 25° C. and quench with saturated aqueous NH4Cl (300 mL). Stir the resulting reaction mixture at room temperature for 20 minutes, then filter, washing the solid with H2O and drying under vacuum filtration for 30 minutes. Slurry the solid in MTBE (200 mL), then filter and rinse with MTBE (50 mL). Dry the recovered solid under vacuum filtration to provide 14.47 g of the title compound as a light-yellow solid.

1. customthe resulting reaction mixture at 80° C. for 3 h
2. temperatureCool
3. customthe reaction to 25° C.
4. customquench with saturated aqueous NH4Cl (300 mL)
5. customthe resulting reaction mixture at room temperature for 20 minutes
6. filtrationfilter
7. washwashing the solid with H2O
8. customdrying under vacuum filtration for 30 minutes
9. filtrationfilter
10. washrinse with MTBE (50 mL)
11. customDry the recovered solid
12. filtrationunder vacuum filtration