反応 #84418

反応方程式

3,4-difluoronitrobenzene

K2CO3

di-n-butylamine

→

title compound

収率 75.1%

N,N-di-n-butyl-2-fluoro-4-nitroaniline

収率 75.1%

溶媒

DMSO

water

反応条件

後処理

1. 1
   温度cooled to rt
2. 2
   抽出extracted with CH2Cl2 (80 mL×3)
3. 3
   乾燥The combined organic phases were dried over anhydrous Na2SO4
4. 4
   濃縮concentrated in vacuo
5. 5
   その他The residue was purified by a silica gel column chromatography (PE/CH2Cl2 (V/V)=10:1)

実験手順

To a solution of 3,4-difluoronitrobenzene (3.18 g, 20 mmol) in DMSO (25 mL) were added K2CO3 (6.08 g, 44 mmol) and di-n-butylamine (2.84 g, 22 mmol) with stirring. The mixture was heated at 90° C. overnight, then cooled to rt, diluted with water (100 mL) and extracted with CH2Cl2 (80 mL×3). The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/CH2Cl2 (V/V)=10:1) to give the title compound as yellow oil (4.03 g, 75%).

出典