反应 #1368

反应方程式

potassium cyanide

ammonium hydroxide

2-methyl-3,4,6-trifluoroaniline

sulfuric acid

sodium nitrite

→

2-methyl-3,4,6-trifluorobenzonitrile

收率 38.2%

溶剂

water

water

反应条件

后处理

1. 1
   温度the mixture is cooled
2. 2
   萃取The mixture is extracted with dichloromethane
3. 3
   干燥the extract is dried over sodium sulfate
4. 4
   浓缩concentrated
5. 5
   其他the residue is purified with column chromatography (silica-gel, dichloromethane:n-hexane=1:4)

实验过程

To 2-methyl-3,4,6-trifluoroaniline (10.6 g) is added a mixture of conc. sulfuric acid (13.8 ml) and water (46 ml) and the mixture is cooled. Thereto an aqueous solution (20 ml) of sodium nitrite (5.5 g) is added dropwise at 0°-5° C. The solution is gradually added to a mixture of copper (II) sulfate 5 hydrate (41 g), potassium cyanide (43 g), ammonium hydroxide (60 ml) and water (260 ml) at 10°-30° C. The mixture is extracted with dichloromethane and the extract is dried over sodium sulfate, concentrated and the residue is purified with column chromatography (silica-gel, dichloromethane:n-hexane=1:4) to give 2-methyl-3,4,6-trifluorobenzonitrile (4.3 g).

来源