反应详情

温度

60 °C

2-Nitro-5-methoxyphenol (prepared from 3-methoxyphenol, R. J. Maleski, Synthetic Communications, 1993, 23, 343-348) (48.5 g, 0.287 mol) dissolved in THF (1.5 L) was hydrogenated at ambient temperature over night with 10% palladium on carbon (10 g) until 20.3 L of hydrogen was consumed. After filtration and evaporation the residue was suspended in degased water (1.7 L) and acetic anhydride (42.5 mL) was added with stirring. The mixture was heated to 60° C. for 1 h and then cooled to room temperature. The volatiles were removed in vacuo and the solid was washed thoroughly with water and dried in vacuo to give brick-red crystals (41.7 g, 80%).

1. customwas consumed
2. filtrationAfter filtration and evaporation the residue
3. additionacetic anhydride (42.5 mL) was added
4. temperaturecooled to room temperature
5. customThe volatiles were removed in vacuo
6. washthe solid was washed thoroughly with water
7. customdried in vacuo