반응 #1994287

반응 방정식

Tin (II) chloride

1,2-dichloro-4-fluoro-5-nitrobenzene

sodium bicarbonate

→

title compound

4,5-Dichloro-2-fluorophenylamine

용매

ethanol

반응 조건

후처리

1. 1
   온도to near reflux during the addition
2. 2
   온도upon cooling
3. 3
   추출extracted with ethyl acetate
4. 4
   세척The organic phase was washed several more times with water
5. 5
   기타dried
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

Tin (II) chloride dehydrate (27.0 g, 119.6 mmol) was dissolved in ethanol and 1,2-dichloro-4-fluoro-5-nitrobenzene (5.0 g, 23.8 mmol) was added dropwise. Temperature rose to near reflux during the addition and was complete upon cooling. The reaction mixture was 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 and concentrated to give the title compound as a yellow solid: 1H NMR (CDCl3): δ 7.17 (d, 1H), 6.84 (d, 1H), 3.78 (br s, 2H).

출처