反应 #465943

反应方程式

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

DMF

phosphorus oxychloride

→

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

收率 79.0%

溶剂

water

反应条件

后处理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   其他reaction for 5 hours
3. 3
   其他The reaction solution obtained
4. 4
   workup.STIRRINGby stirring for 1 hour
5. 5
   过滤Thereafter, the precipitate was collected by filtration
6. 6
   洗涤washed with a mixture of ethanol/water (1:1)

实验过程

Into a three-necked flask, 124.6 g of [N,N-bis(3,4-dimethylphenyl)amino]benzene and 35.5 ml of DMF were placed, and 84.4 ml of phosphorus oxychloride was added dropwise thereto with stirring while cooling with ice water. After the addition was completed, the mixture solution was heated to 95° C. to carry out reaction for 5 hours. The reaction solution obtained was poured into 4 liters of warm water, followed by stirring for 1 hour. Thereafter, the precipitate was collected by filtration, and washed with a mixture of ethanol/water (1:1) to obtain 4-[N,N-bis(3,4-dimethylphenyl)amino]benzaldehyde in an amount of 107.6 g (yield: 79.0%).

来源