反应详情

温度

0 °C

To a 0° C. cooled stirred solution of 5-nitro-2,3′-bipyridin-6-amine (4.8 g, 22.2 mmol) in DMF (50 mL), N-bromosuccinimide (4.75 g, 26.7 mmol) was added in portions. After stirring at room temperature for 16 h, the solvent was removed under reduced pressure. The crude residue was solved with ethyl acetate and washed with saturated potassium carbonate aqueous solution. The organic layer was washed with brine, dried (MgSO4) and evaporated. The residue was purified by silica gel flash chromatography (95:5 dichloromethane/methanol) to give the title compound (6.6 g, 100%) as a solid.

1. additionwas added in portions
2. customthe solvent was removed under reduced pressure
3. washwashed with saturated potassium carbonate aqueous solution
4. washThe organic layer was washed with brine
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe residue was purified by silica gel flash chromatography (95:5 dichloromethane/methanol)