反应详情

温度

90 °C

4-bromo-2-methyl-pyridine (5 g, 29.07 mmol), 2-[(E)-(1-cyano-1-methyl-ethyl)azo]-2-methyl-propanenitrile (954.7 mg, 5.814 mmol) and N-bromosuccinimide (7.244 g, 40.70 mmol) were added to fluorobenzene (8 mL) and the mixture heated to 90° C. for 1 hour. Reaction mixture was purified by filtering through a silica gel pad and eluting with 50% diethylether/petroleum ether. Product fractions were combined and concentrated in vacuo to give the crude sub-title product (7.294 g, assumed 100% yield). 1H NMR (400.0 MHz, DMSO-d6) δ 4.52 (s, 2H), 7.42 (d, 1H), 7.65 (s, 1H) and 8.42 (d, 1H) ppm.

1. customReaction mixture
2. customwas purified
3. filtrationby filtering through a silica gel pad
4. washeluting with 50% diethylether/petroleum ether
5. concentrationconcentrated in vacuo