反应 #1869215

反应方程式

hydrogen

2-Nitro-5-methoxyphenol

THF

→

crystals

收率 80.0%

N-(2-Hydroxy-4 methoxyphenyl)acetamide

收率 80.0%

反应条件

后处理

1. 1
   其他was consumed
2. 2
   过滤After filtration and evaporation the residue
3. 3
   workup.ADDITIONacetic anhydride (42.5 mL) was added
4. 4
   温度cooled to room temperature
5. 5
   其他The volatiles were removed in vacuo
6. 6
   洗涤the solid was washed thoroughly with water
7. 7
   其他dried in vacuo

实验过程

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 degassed 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%).

来源