反应详情

To a mixture of 4-fluoro-3-methoxyaniline (2.0 g, 14.2 mmol) in CH2Cl2 (20 mL) at 0° C. was added 1.0 M solution of BBr3 in CH2Cl2 (40 mL). It was stirred overnight, at which time the temperature was raised to room temperature. To it was added MeOH and the solvents were removed under reduced pressure. To the residue was added water, basified with saturated NaHCO3, and extracted with EtOAc. Extracts were washed with brine, dried over MgSO4, and concentrated under reduced pressure to afford 5-amino-2-fluorophenol as solid (1.3 g, 73%). 1H NMR (300 MHz, DMSO-d6) δ 9.26 (s, 1H), 6.81 (dd, 1H), 6.34 (dd, 1H), 6.04 (dd, 1H), 4.63 (br, 2H).

1. customthe solvents were removed under reduced pressure
2. additionTo the residue was added water
3. extractionextracted with EtOAc
4. washExtracts were washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated under reduced pressure