反応 #465943

反応方程式

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

DMF

phosphorus oxychloride

→

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

収率 79.0%

溶媒

water

反応条件

後処理

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

実験手順

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%).

出典