تفاعل #2850

معادلة التفاعل

4-amino-3-methyl benzonitrile

benzophenone

p-toluenesulfonic acid

→

title compound

المردود 90.3%

4-(Benzhydrylidene-amino)-3-methyl-benzonitrile

المردود 90.3%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction vessel is fitted with a Dean-Stark trap
2. 2
   درجة الحرارةthe solution is heated
3. 3
   درجة الحرارةat reflux
4. 4
   درجة الحرارةthe solution is cooled to ambient temperatures
5. 5
   تركيزThe solution is concentrated
6. 6
   أخرىThe crude material is purified by column chromatography
7. 7
   غسيلeluting with a gradient of 3% EtOAc/hexanes to 10% EtOAc/hexanes

الإجراء التجريبي

To a solution of 4-amino-3-methyl benzonitrile (1.20 g, 9.08 mmol) in 75 mL of toluene is added benzophenone (1.74 g, 9.53 mmol) and p-toluenesulfonic acid (0.43 g, 2.1 mmol). The reaction vessel is fitted with a Dean-Stark trap and the solution is heated at reflux. After 24 h, the solution is cooled to ambient temperatures. The solution is concentrated. The crude material is purified by column chromatography eluting with a gradient of 3% EtOAc/hexanes to 10% EtOAc/hexanes. The title compound (2.43 g, 8.2 mmol) is obtained as an oil.

المصدر