反应 #325875

反应方程式

sulfuric acid

Sodium nitrate

2-Bromo-phenol

→

2-bromo-6-nitro-phenol

收率 42.8%

溶剂

water

ethyl acetate

反应条件

后处理

1. 1
   其他was kept below 25° C
2. 2
   洗涤The mixture was washed with water and saturated brine
3. 3
   干燥dried over anhydrous magnesium sulfate
4. 4
   过滤filtered
5. 5
   浓缩the filtrate was concentrated under reduced pressure
6. 6
   其他The resulting residue was purified by silica gel column chromatography

实验过程

A solution of 60 mL of concentrated sulfuric acid diluted with 186 mL of water was cooled to room temperature. Sodium nitrate (79.2 g, 0.93 mol) was added to the solution. 2-Bromo-phenol 1a (60 mL, 0.52 mol) was added dropwise at such a rate that the reaction temperature was kept below 25° C. The reaction mixture was stirred at room temperature for 2 hours. The precipitate was dissolved in 320 mL of ethyl acetate. The mixture was washed with water and saturated brine, dried over anhydrous magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound 2-bromo-6-nitro-phenol 1b (48.2 g, yield 42.8%) as a yellow solid.

来源