تفاعل #1368

معادلة التفاعل

potassium cyanide

ammonium hydroxide

2-methyl-3,4,6-trifluoroaniline

sulfuric acid

sodium nitrite

→

2-methyl-3,4,6-trifluorobenzonitrile

المردود 38.2%

المذيبات

water

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture is cooled
2. 2
   استخلاصThe mixture is extracted with dichloromethane
3. 3
   تجفيفthe extract is dried over sodium sulfate
4. 4
   تركيزconcentrated
5. 5
   أخرىthe residue is purified with column chromatography (silica-gel, dichloromethane:n-hexane=1:4)

الإجراء التجريبي

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).

المصدر