Réaction #465943

Équation de réaction

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

DMF

phosphorus oxychloride

→

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

Rendement 79.0%

Solvants

water

Conditions de réaction

Traitement

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

Mode opératoire

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%).

Source