反应详情

To a solution of 6-fluoro-1-methyl-1H-pyrrolo[2,3-b]pyridine (257.3 g, 1.71 mol) in DCM (3.86 L) is added N-bromosuccinimide (320.3 g; 1.80 mol) in five portions over 30 minutes. The mixture is stirred without heating or cooling overnight, then filtered and concentrated to about 1 L. This is purified by column chromatography on silica, eluting with 0 to 30% EtOAc in isohexane. The appropriate fractions are evaporated to give the product as an off white solid (391.3 g, 1.7 mol). 1H-NMR (400 MHz, CDCl3): δ 7.91-7.87 (m, 1H), 7.15 (s, 1H), 6.77 (d, 1H), 3.81 (s, 3H).

1. temperaturewithout heating
2. temperaturecooling overnight
3. filtrationfiltered
4. concentrationconcentrated to about 1 L
5. customThis is purified by column chromatography on silica
6. washeluting with 0 to 30% EtOAc in isohexane
7. customThe appropriate fractions are evaporated