反应详情

A mixture of 6-cyano-3-picoline (1.32 g, 11.19 mmol), benzoylperoxide (0.54 g, 2.24 mmol), and N-bromosuccinimide (2.8 g, 15.7 mmol) in carbontetrachloride (30 mL) was heated at reflux for 2 h. The resulting suspension was filtered and the filtrate diluted with dichloromethane (400 mL), washed with a saturated sodium bicarbonate solution, dried over magnesium sulfate, and concentrated in vacuo. The residue was purified by column chromatography (EtOAc:n-hexane, 1:9) to give the title compound as a yellow oil (1.12 g, 51%).

1. temperaturewas heated
2. temperatureat reflux for 2 h
3. filtrationThe resulting suspension was filtered
4. additionthe filtrate diluted with dichloromethane (400 mL)
5. washwashed with a saturated sodium bicarbonate solution
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by column chromatography (EtOAc:n-hexane, 1:9)