反应详情

温度

60 °C

A mixture of 5-bromo-4,6-dimethyl-pyridin-3-amine (500 mg, 2.49 mmol) and nitrosyl tetrafluoroborate (445 mg, 3.73 mmol) in 1-butyl-3-methylimidazolium tetrafluoroborate (9.48 mL, 49.74 mmol) was heated at 60° C. for 2 hours (caution: exothermic). The reaction mixture was diluted with ethyl acetate (50 mL) and washed with water (2×20 mL), and then saturated aqueous sodium bicarbonate (20 mL). The organic layer was separated, dried over sodium sulfate, filtered and concentrated in vacuo to provide a residue that was purified by flash chromatography (4 g, Silica, 0-50% ethyl acetate in heptane). Desired fractions were combined and evaporated in vacuo to afford the title compound as pale yellow oil (220 mg, 43%), which was used in the next step without further purification.

1. washwashed with water (2×20 mL)
2. customThe organic layer was separated
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customto provide a residue that
7. customwas purified by flash chromatography (4 g, Silica, 0-50% ethyl acetate in heptane)
8. customevaporated in vacuo