反应详情

To a solution of 5-amino-2-chloro-phenol (15.85 g, 110.4 mmol) in dichloromethane (300 ml) and MeOH (150 ml) was added tetrabutylammonium tribromide (58.6 g, 121.4 mmol). The mixture was stirred at room temperature for 20 minutes, and then was partitioned between saturated aqueous Na2SO3 and Et2O. The organic layer was separated, washed with water and brine, dried over MgSO4, filtered and concentrated to dryness under reduced pressure. Purification of the residue by flash chromatography (hex:EtOAc/7:3) gave 5-amino-4-bromo-2-chloro-phenol (4.38 g, 18%) as a white solid.

1. customwas partitioned between saturated aqueous Na2SO3 and Et2O
2. customThe organic layer was separated
3. washwashed with water and brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated to dryness under reduced pressure
7. customPurification of the residue by flash chromatography (hex:EtOAc/7:3)