Reaktion #367328

Reaktionsgleichung

7-methoxy-1-tetralone

dimethyl amine

→

amber oil

Ausbeute 87.5%

1-Dimethylamino-7-methoxy-3,4-dihydronaphthalene

Ausbeute 87.5%

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile maintaining a reaction temperature of ≤10° C
2. 2
   Sonstigethe ice bath is removed
3. 3
   Sonstigeto reach RT
4. 4
   FiltrationThe solids are filtered
5. 5
   Waschenwashed with dry toluene
6. 6
   Sonstigethe filtrate evaporated in vacuo

Vorschrift

A solution of titanium tetrachloride (53.8 g, 31.2 ml) in dry toluene (200 ml) is added over a period of 45 minutes to a stirred solution of 7-methoxy-1-tetralone (100.5 g) and dimethyl amine (171 g) in dry toluene (2 l) while maintaining a reaction temperature of ≤10° C. When the addition of the titanium is complete, the ice bath is removed and the solution allowed to reach RT. The solution is stirred at RT for 3 hours. The solids are filtered, washed with dry toluene and the filtrate evaporated in vacuo, yielding 101.4 g of an amber oil which is used in the next step without further treatment.

Quelle