Reaktion #486874

Reaktionsgleichung

sodium hydride

1,2-dimethoxyethane

4-(N,N-diphenylamino) benzaldehyde

→

vinyltriphenylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe mixture was reacted for 4 hours at 70° C
2. 2
   TemperaturThe temperature was raised to 70° C.
3. 3
   Sonstigethe mixture was reacted for 5 hours
4. 4
   FiltrationThe reaction solution was filtered
5. 5
   Extraktionan ether extract of the precipitate
6. 6
   Waschenthe filtrate were washed in water
7. 7
   Sonstigethe ether was removed
8. 8
   Sonstigethe reaction mixture was obtained
9. 9
   SonstigeThis was recrystallized from ethanol

Vorschrift

14.6 g of sodium hydride and 700 mL of 1,2-dimethoxyethane were placed in a three-neck flask, and while stirring at room temperature, 130.8 g of tetramethylphosphonium bromide was added. After adding one drop of anhydrous ethanol, the mixture was reacted for 4 hours at 70° C. Then 100 g of 4-(N,N-diphenylamino) benzaldehyde was added to the mixture. The temperature was raised to 70° C., and the mixture was reacted for 5 hours. The reaction solution was filtered, and an ether extract of the precipitate and the filtrate were washed in water. Next, the ether solution was dehydrated with calcium chloride, the ether was removed, and the reaction mixture was obtained. This was recrystallized from ethanol, and a needle-form, lemon-yellow vinyltriphenylamine was obtained. The yield was 83.4 g (yield rate of 84.0%).

Quelle