反应详情

Add a solution of methyl 2-nitro-4-trifluoromethylbenzoate (106 g, 425 mmol) in ethyl acetate (2.2 L) to a slurry of 10% palladium on carbon (11.0 g) in ethyl acetate (200 mL) and stir the suspension at room temperature under an atmosphere of hydrogen at 60 psi for 3 h. Filter the suspension through a pad of Celite® and wash the pad with additional ethyl acetate. Remove the solvents under reduced pressure and purify the residue by column chromatography on silica gel, eluting with isohexane/ethyl acetate (9:1), to provide the title compound as a white crystalline solid (84 g, 95%). 1H NMR (300 MHz, CD3OD) δ 7.93 (d, J=8.48 Hz, 1H), 7.06 (s, 1H), 6.78 (s, 1H), 4.86 (s, 3H), 3.89 (s, 3H).

1. filtrationFilter the suspension through a pad of Celite®
2. washwash the pad with additional ethyl acetate
3. customRemove the solvents under reduced pressure
4. custompurify the residue by column chromatography on silica gel
5. washeluting with isohexane/ethyl acetate (9:1)