反应 #2075715

反应方程式

Tin (II) chloride dihydrate

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

sodium bicarbonate

→

title compound

收率 73.9%

4-Chloro-2,5-difluorophenylamine

收率 73.9%

溶剂

ethyl acetate

反应条件

后处理

1. 1
   萃取extracted with ethyl acetate
2. 2
   洗涤The organic phase was washed several more times with water
3. 3
   其他dried
4. 4
   过滤filtered
5. 5
   浓缩concentrated
6. 6
   其他purified by flash chromatography on silica gel (hexane/diethyl ether)

实验过程

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).

来源