反应详情

温度

60 °C

2-Nitro-5-methoxyphenol (R. J. Maleski, Synthetic Communications, 23(3), 343-348 (1993)) (48.5 g, 0.287 mol) dissolved in tetrahydrofuran (THF) (1.5 L) was hydrogenated at ambient temperature over night with 10% Pd/C (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. The isolated 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
5. washThe isolated solid was washed thoroughly with water
6. customdried in vacuo