Reaktion #1119449

Reaktionsgleichung

2-cyano-1,2,3,4,8,9,10,10a-octahydronaphth[1,8-cd]azepine

→

1,2,3,4,8,9,10,10a-octahydronaphth[1,8-cd]azepine

Ausbeute 70.0%

Lösungsmittel

acetic acid

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 20 hours
2. 2
   EinengenThe solution was concentrated to a small volume, approximately 30 ml of water
3. 3
   workup.ADDITIONwas added
4. 4
   Sonstigeneutral materials were removed by extraction with ether
5. 5
   workup.ADDITIONThe aqueous layer was made basic by addition of NaOH
6. 6
   Extraktionthe product was extracted with ether
7. 7
   SonstigeAfter evaporation of the ether

Vorschrift

A solution of 1.3 g (6.1 mmol) of 2-cyano-1,2,3,4,8,9,10,10a-octahydronaphth[1,8-cd]azepine, an intermediate of Formula 8 prepared, for example, as described in Preparation 8A, in a mixture of 40 ml of acetic acid and 40 ml of 20% hydrochloric acid, was kept at reflux for 20 hours. The solution was concentrated to a small volume, approximately 30 ml of water was added and neutral materials were removed by extraction with ether. The aqueous layer was made basic by addition of NaOH, and the product was extracted with ether. After evaporation of the ether, 0.8 g of 1,2,3,4,8,9,10,10a-octahydronaphth[1,8-cd]azepine was obtained as an oil (HCl salt, mp 207°-209° C.).

Quelle