反应 #62037

反应方程式

1-(2,5-dichloro-phenoxy)-2-fluoro-4-nitro-benzene

tin chloride

sodium bicarbonate

→

4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylamine

溶剂

ethanol

反应条件

后处理

1. 1
   温度to cool
2. 2
   workup.ADDITIONpoured into ice
3. 3
   萃取extracted with ethyl acetate
4. 4
   洗涤The organic phase was thoroughly washed with brine
5. 5
   其他dried
6. 6
   workup.ADDITIONtreated with anhydrous sodium sulfate
7. 7
   其他Evaporation of the solvent
8. 8
   workup.WAITleft a yellow oily product which
9. 9
   其他was used for the next step without further purification

实验过程

A mixture of 1-(2,5-dichloro-phenoxy)-2-fluoro-4-nitro-benzene (0.5 g, 1.7 mmol) and tin chloride (1.57 g, 8.3 mmol) in 30 ml of anhydrous ethanol was heated to 70° C. under argon and stirred for 4 hours. The solution was allowed to cool and then poured into ice. The solution was made slightly basic (pH 7-8) by addition of saturated aqueous sodium bicarbonate solution, then extracted with ethyl acetate. The organic phase was thoroughly washed with brine and dried treated with anhydrous sodium sulfate. Evaporation of the solvent left a yellow oily product which was used for the next step without further purification.

来源