反应详情

In 290 ml of acetic acid were dissolved 26.4 g (0.168 mole) of 2-fluoro-6-nitrophenol and 17.2 g (0.168 mole) of acetic anhydride, and 3.0 g of 5 % palladium carbon was added thereto. Hydrogen gas was passed through the mixture, with stirring, at room temperature for 2 hours. After the reaction mixture had been filtered and the filtrate concentrated under reduced pressure, the residue was extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was applied to silica gel column chromatography (the eluent used was a mixture of ethyl acetate : toluene = 1 : 2) to obtain 25.9 g of 2-acetylamino-6-fluorophenol as brown crystals.

1. additionwas added
2. filtrationAfter the reaction mixture had been filtered
3. concentrationthe filtrate concentrated under reduced pressure
4. extractionthe residue was extracted with ethyl acetate
5. washThe ethyl acetate layer was washed with water
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was removed under reduced pressure
8. additiona mixture of ethyl acetate