반응 #367328

반응 방정식

7-methoxy-1-tetralone

dimethyl amine

→

amber oil

수율 87.5%

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

수율 87.5%

용매

toluene

toluene

반응 조건

후처리

1. 1
   온도while maintaining a reaction temperature of ≤10° C
2. 2
   기타the ice bath is removed
3. 3
   기타to reach RT
4. 4
   여과The solids are filtered
5. 5
   세척washed with dry toluene
6. 6
   기타the filtrate evaporated in vacuo

실험 절차

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.

출처