反応 #465944

反応方程式

4-[N,N-bis(3,4-dimethylphenyl)amino]benzaldehyde

trimethylphosphonium bromide

sodium hydride

→

4-[N,N-bis(3,4-dimethylphenyl)amino]styrene

収率 85.0%

溶媒

1,2-dimethoxyethane

反応条件

後処理

1. 1
   その他reaction at 700° C. for 5 hours
2. 2
   ろ過followed by filtration
3. 3
   その他to collect a cake
4. 4
   抽出The cake was extracted with ether
5. 5
   洗浄washed with water
6. 6
   その他the ether was removed
7. 7
   その他to obtain a crude product
8. 8
   その他After twice recrystallized from ethanol

実験手順

Into a three-necked flask, 12.1 g of sodium hydride and 580 ml of 1,2-dimethoxyethane were placed, and 108.5 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, 100.0 g of 4-[N,N-bis(3,4-dimethylphenyl)amino]benzaldehyde was added to the reaction mixture, to carry out reaction at 700° C. for 5 hours, followed by filtration to collect a cake. The cake was extracted with ether and the extract was put together with the filtrate and washed with water. Then, the ether solution was dehydrated with calcium chloride, and thereafter the ether was removed to obtain a crude product. After twice recrystallized from ethanol, acicular 4-[N,N-bis(3,4-dimethylphenyl)amino]styrene was obtained in an amount of 84.5 g (yield: 85.0%).

出典