تفاعل #341443

معادلة التفاعل

2-chloro-5-nitrobenzonitrile

tributyl tin azide

azide

→

product 10

المردود 127.7%

5-(2-chloro-5-nitrophenyl)-2H-tetrazole

المردود 127.7%

المذيبات

toluene

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThen the mixture is heated
2. 2
   درجة الحرارةunder reflux for a further 5 hours
3. 3
   تركيزThe mixture is then concentrated
4. 4
   workup.ADDITION10 mL of HCl 2 N in Et2O are added
5. 5
   أخرىthe precipitate formed
6. 6
   ترشيحis filtered
7. 7
   غسيلwashed with pentane and diethyl ether

الإجراء التجريبي

137 mg (0.750 mmol, 1 eq.) of 2-chloro-5-nitrobenzonitrile are dissolved in 8 mL of toluene, and 411 μl (1.5 mmol, 2 eq.) of tributyl tin azide are added to the reaction mixture. Then the mixture is heated under reflux of the toluene for one night. As the reaction is incomplete, 205 μl (0.75 mmol, 1 eq.) of azide are again added and the mixture is stirred under reflux for a further 5 hours. The mixture is then concentrated and 10 mL of HCl 2 N in Et2O are added, the precipitate formed is filtered and washed with pentane and diethyl ether. 216 mg of product 10 are obtained (yield=64%).

المصدر