反应详情

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).

1. temperaturethe mixture is cooled
2. extractionThe mixture is extracted with dichloromethane
3. dry with materialthe extract is dried over sodium sulfate
4. concentrationconcentrated
5. customthe residue is purified with column chromatography (silica-gel, dichloromethane : n-hexane =1 : 4)