反应 #319829

反应方程式

2,4,5-trifluoro-3-methyl-6-methylthiomethylaniline

→

2,4,5-trifluoro-3,6-dimethylaniline

收率 69.7%

溶剂

ethanol

反应条件

后处理

1. 1
   过滤After Raney nickel is filtered off
2. 2
   浓缩the filtrate is concentrated
3. 3
   workup.ADDITIONdiluted with water
4. 4
   萃取extracted with dichloromethane
5. 5
   洗涤the extract is washed with water
6. 6
   其他dried
7. 7
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
8. 8
   其他the residue is purified by silica-gel column-chromatography (dichloromethane: n-hexane =1:1)

实验过程

To 2,4,5-trifluoro-3-methyl-6-methylthiomethylaniline (10.67 g) are added ethanol (300 ml) and Raney nickel (100 g, wet) and the mixture is stirred at room temperature for 30 minutes. After Raney nickel is filtered off, the filtrate is concentrated, diluted with water, extracted with dichloromethane, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and the residue is purified by silica-gel column-chromatography (dichloromethane: n-hexane =1:1) to give 2,4,5-trifluoro-3,6-dimethylaniline (5.89 g), as yellow crystals.

来源