反应详情

A solution of 3-(1-(2,3-difluorophenyl)-1H-imidazo[4,5-c]pyridin-2-yl)pyridin-2-amine (2.4 g, 7.43 mmol) in acetonitrile (70 mL) was treated with N-bromosuccinimide (1.45 g, 18.17 mmol) at 0° C. and the reaction mixture stirred for 30 min. reaction mixture was treated with saturated aq. NaHCO3 solution (150 mL), stirred for 30 min, and the resulting precipitate filtered and dissolved in CHCl3 (200 mL). The combined organics were washed with water (3×70 mL), brine (70 mL), and dried (Na2SO4). Filtration and evaporation of solvent in vacuo gave a solid, which was purified by silica gel chromatography (4% methanol/chloroform) to give 5-bromo-3-(1-(2,3-difluorophenyl)-1H-imidazo[4,5-c]pyridin-2-yl)pyridin-2-amine (2.2 g, 75% yield) as a light yellow solid; LC-MS: 402.0, 404.0 (M+H).

1. customreaction mixture
2. stirringstirred for 30 min
3. filtrationthe resulting precipitate filtered
4. dissolutiondissolved in CHCl3 (200 mL)
5. washThe combined organics were washed with water (3×70 mL), brine (70 mL)
6. dry with materialdried (Na2SO4)
7. filtrationFiltration and evaporation of solvent in vacuo
8. customgave a solid, which
9. customwas purified by silica gel chromatography (4% methanol/chloroform)