Реакция #465943

Уравнение реакции

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

DMF

phosphorus oxychloride

→

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

Выход 79.0%

Растворители

water

Условия реакции

Обработка

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

Методика

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%).

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