반응 #2075715

반응 방정식

Tin (II) chloride dihydrate

1-chloro-2,5-difluoro-4-nitrobenzene

sodium bicarbonate

→

title compound

수율 73.9%

4-Chloro-2,5-difluorophenylamine

수율 73.9%

용매

ethyl acetate

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   세척The organic phase was washed several more times with water
3. 3
   기타dried
4. 4
   여과filtered
5. 5
   농축concentrated
6. 6
   기타purified by flash chromatography on silica gel (hexane/diethyl ether)

실험 절차

Tin (II) chloride dihydrate (15.5 g, 68.7 mmol) was dissolved in ethyl acetate (50 mL) and 1-chloro-2,5-difluoro-4-nitrobenzene (2.65 g, 13.7 mmol) was added dropwise. The reaction mixture was then stirred at 70° C. for 1 h. The reaction mixture was then carefully added to saturated aqueous sodium bicarbonate and then extracted with ethyl acetate. The organic phase was washed several more times with water, dried, filtered, concentrated and purified by flash chromatography on silica gel (hexane/diethyl ether) to give the title compound as a white solid (1.65 g, 73.9% yield): 1H NMR (CDCl3): δ 7.02 (dd, 1H), 6.57 (dd, 1H), 3.81 (br s, 2H).

출처