反应 #465944

反应方程式

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

trimethylphosphonium bromide

sodium hydride

→

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

收率 85.0%

溶剂

1,2-dimethoxyethane

反应条件

后处理

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

实验过程

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%).

来源