反应详情

To a solution of 5-bromo-2-fluoro-pyridine-3-carbaldehyde (2) (20.0 g, 98.0 mmol) in 1:1 MeOH—H2O (250 mL) was added hydroxylamine hydrochloride (7.52 g, 108 mmol) and sodium carbonate (11.4 g, 108 mmol). The reaction mixture was stirred at rt for 1 hour. The solvent was evaporated in vacuo and the residue diluted with H2O (200 mL) and EtOAc (200 mL). The organic phase was separated, dried (Na2SO4), filtered and the solvent evaporated in vacuo. The product was obtained as a light pink solid (21.0 g, 93%); Rf: 0.4 (10% EtOAc-pet ether).

1. customThe solvent was evaporated in vacuo
2. additionthe residue diluted with H2O (200 mL) and EtOAc (200 mL)
3. customThe organic phase was separated
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customthe solvent evaporated in vacuo