反应详情

Nitrosonium tetrafluoroborate (300 mg, 2.58 mmol) was added to a suspension of 3-amino-5-bromopyridine-2-carboxamide (466 mg, 2.15 mmol) in DCM (30 mL) and the mixture stirred at room temperature for 16 h. The solvent was removed in vacuo and toluene (30 mL) was added and the mixture heated to reflux for 2 h. After cooling to room temperature the solvent was removed in vacuo and the crude slurried in DCM (10 mL), filtered, washed with DCM and dried in vacuo at 40° C. to give 3-fluoro-5-bromopyridine-2-carboxamide which was used directly without further purification.

1. customThe solvent was removed in vacuo and toluene (30 mL)
2. additionwas added
3. temperaturethe mixture heated
4. temperatureto reflux for 2 h
5. temperatureAfter cooling to room temperature the solvent
6. customwas removed in vacuo
7. filtrationfiltered
8. washwashed with DCM
9. customdried in vacuo at 40° C.