반응 #465942

반응 방정식

4-(N,N-diphenylamino)benzaldehyde

trimethylphosphonium bromide

sodium hydride

1,2-dimethoxyethane

→

vinyltriphenylamine

수율 84.0%

반응 조건

후처리

1. 1
   온도the temperature was raised to 70° C.
2. 2
   기타reaction for 5 hours
3. 3
   기타The resulting reaction solution
4. 4
   여과was filtered
5. 5
   추출the filtrate and an ether-extract of the precipitate
6. 6
   세척washed with water
7. 7
   기타was removed
8. 8
   기타to obtain a crude
9. 9
   기타reaction product
10. 10
    기타After recrystallized from ethanol

실험 절차

Into a three-necked flask, 14.6 g of sodium hydride and 700 ml of 1,2-dimethoxyethane were placed, and 130.8 g of trimethylphosphonium bromide was added thereto with stirring at room temperature. Next, after a drop of absolute alcohol was added, the reaction was allowed to proceed at 70° C. for 4 hours. Then, 100 g of 4-(N,N-diphenylamino)benzaldehyde was added thereto, and the temperature was raised to 70° C. to carry out reaction for 5 hours. The resulting reaction solution was filtered, and the filtrate and an ether-extract of the precipitate were put together and washed with water. Then, the ether solution was dehydrated with calcium chloride, and ether was removed to obtain a crude reaction product. After recrystallized from ethanol, acicular pale yellow vinyltriphenylamine was obtained in an amount of 83.4 g (yield: 84.0%).

출처