반응 #84418

반응 방정식

3,4-difluoronitrobenzene

K2CO3

di-n-butylamine

→

title compound

수율 75.1%

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

수율 75.1%

용매

DMSO

water

반응 조건

후처리

1. 1
   온도cooled to rt
2. 2
   추출extracted with CH2Cl2 (80 mL×3)
3. 3
   건조The combined organic phases were dried over anhydrous Na2SO4
4. 4
   농축concentrated in vacuo
5. 5
   기타The residue was purified by a silica gel column chromatography (PE/CH2Cl2 (V/V)=10:1)

실험 절차

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%).

출처