反应详情

In a 500 ml, 4-necked round-bottomed flask equipped with an overhead mechanical stirrer, a thermometer/adaptor, a reflux condensor and a funnel was added 2,6-di-(4-benzocyclobutenoxy)benzonitrile followed by 260 ml of anhydrous diethyl ether. The resultant mixture was placed in an ice bath and stirred under a nitrogen atmosphere. When the internal temperature reached 0° C., lithium aluminum hydride was added through the attached funnel in 3 portions (0.69 g, 0.96 g, 0.50 g), each addition followed by washing the funnel with about 10 ml Et2O, over a period of 15 minutes. The resulting mixture was stirred at 0° C. for 20 minutes, then the ice bath was removed and the mixture. was allowed to warm to room temperature. The reaction mixture was then refluxed gently for 17 hours.

1. customIn a 500 ml, 4-necked round-bottomed flask equipped with an overhead mechanical stirrer
2. customreached 0° C.
3. additioneach addition
4. washby washing the funnel with about 10 ml Et2O
5. stirringThe resulting mixture was stirred at 0° C. for 20 minutes
6. customthe ice bath was removed
7. temperatureThe reaction mixture was then refluxed gently for 17 hours