反应详情

To a solution of acetic acid 6-fluoro-3-nitro-2-phenylaminobenzyl ester (3.2 g, 10.5 mmol) in EtOAc (50 mL) was added palladium on carbon (600 mg, 10% by wt) and the reaction mixture stirred at RT under an atmosphere of hydrogen for 16 h. The reaction mixture was filtered and the filtrate concentrated in vacuo. The resultant residue was subjected to flash chromatography (SiO2, eluting with 0-100% DCM in cyclohexane) to give the title compound as a brown solid (2.3 mg, 80%). 1H NMR 400 MHz δ (CDCl3): 7.22-7.15 (2H, m), 6.86 (1H, t, J=8.9 Hz), 6.81 (1H, tt, J=7.4, 1.0 Hz), 6.78-6.71 (1H, m), 6.63-6.58 (2H, m), 6.43 (1H, br s), 5.10 (2H, d, J=1.9 Hz), 3.72 (2H, br s), 1.99 (3H, s).

1. filtrationThe reaction mixture was filtered
2. concentrationthe filtrate concentrated in vacuo
3. washThe resultant residue was subjected to flash chromatography (SiO2, eluting with 0-100% DCM in cyclohexane)