Reaktion #6289

Reaktionsgleichung

2,6-di-(4-benzocyclobutenoxy)benzonitrile

lithium aluminum hydride

→

2,6-di-(4-benzocyclobutenoxy)benzylamine

Lösungsmittel

diethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeIn a 500 ml, 4-necked round-bottomed flask equipped with an overhead mechanical stirrer
2. 2
   Sonstigereached 0° C.
3. 3
   workup.ADDITIONeach addition
4. 4
   Waschenby washing the funnel with about 10 ml Et2O
5. 5
   workup.STIRRINGThe resulting mixture was stirred at 0° C. for 20 minutes
6. 6
   Sonstigethe ice bath was removed
7. 7
   TemperaturThe reaction mixture was then refluxed gently for 17 hours

Vorschrift

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 anitrogen 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.

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