반응 #465943

반응 방정식

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

DMF

phosphorus oxychloride

→

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

수율 79.0%

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   기타reaction for 5 hours
3. 3
   기타The reaction solution obtained
4. 4
   workup.STIRRINGby stirring for 1 hour
5. 5
   여과Thereafter, the precipitate was collected by filtration
6. 6
   세척washed with a mixture of ethanol/water (1:1)

실험 절차

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%).

출처