反応 #2075715

反応方程式

Tin (II) chloride dihydrate

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

sodium bicarbonate

→

title compound

収率 73.9%

4-Chloro-2,5-difluorophenylamine

収率 73.9%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   洗浄The organic phase was washed several more times with water
3. 3
   その他dried
4. 4
   ろ過filtered
5. 5
   濃縮concentrated
6. 6
   その他purified by flash chromatography on silica gel (hexane/diethyl ether)

実験手順

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).

出典