反应详情

A mixture of 5-methylthiophene-2-carbonitrile (9.9 g, 80.5 mmol), benzoylperoxide (0.23 g, 0.95 mmol), and N-bromosuccinimide (15 g, 84.3 mmol) in carbontetrachloride (200 mL) was heated at reflux for 6 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, 1:4) to give the title compound as a yellow oil (14.0 g, 86%).

1. temperaturewas heated
2. temperatureat reflux for 6 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, 1:4)