Реакция #1368

Уравнение реакции

potassium cyanide

ammonium hydroxide

2-methyl-3,4,6-trifluoroaniline

sulfuric acid

sodium nitrite

→

2-methyl-3,4,6-trifluorobenzonitrile

Выход 38.2%

Растворители

water

water

Условия реакции

Обработка

1. 1
   Температураthe mixture is cooled
2. 2
   ЭкстракцияThe mixture is extracted with dichloromethane
3. 3
   Сушкаthe extract is dried over sodium sulfate
4. 4
   Концентрированиеconcentrated
5. 5
   Другоеthe residue is purified with column chromatography (silica-gel, dichloromethane:n-hexane=1:4)

Методика

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).

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