تفاعل #367328

معادلة التفاعل

7-methoxy-1-tetralone

dimethyl amine

→

amber oil

المردود 87.5%

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

المردود 87.5%

المذيبات

toluene

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwhile maintaining a reaction temperature of ≤10° C
2. 2
   أخرىthe ice bath is removed
3. 3
   أخرىto reach RT
4. 4
   ترشيحThe solids are filtered
5. 5
   غسيلwashed with dry toluene
6. 6
   أخرىthe filtrate evaporated in vacuo

الإجراء التجريبي

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.

المصدر