反応 #1994287

反応方程式

Tin (II) chloride

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

sodium bicarbonate

→

title compound

4,5-Dichloro-2-fluorophenylamine

溶媒

ethanol

反応条件

後処理

1. 1
   温度to near reflux during the addition
2. 2
   温度upon cooling
3. 3
   抽出extracted with ethyl acetate
4. 4
   洗浄The organic phase was washed several more times with water
5. 5
   その他dried
6. 6
   ろ過filtered
7. 7
   濃縮concentrated

実験手順

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).

出典