反应 #465941

ord-17534e2ccb6c45a8bd9e00cfe1233de6

反应方程式

c1ccc(N(c2ccccc2)c2ccccc2)cc1
triphenylamine
CN(C)C=O
DMF
O=P(Cl)(Cl)Cl
phosphorus oxychloride
O=Cc1ccc(N(c2ccccc2)c2ccccc2)cc1
4-(N,N-diphenylamino)benzaldehyde
收率 81.0%

溶剂

反应条件

温度
95°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他reaction for 5 hours
  2. 2
    其他The reaction solution obtained
  3. 3
    workup.STIRRINGby stirring for 1 hour
  4. 4
    其他Thereafter, the precipitate formed
  5. 5
    过滤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, 101.4 g of triphenylamine and 35.5 ml of DMF (dimethylformamide) were placed, and 84.4 ml of phosphorus oxychloride was added dropwise thereto with stirring while cooling with ice water, and then the temperature was raised 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 formed was collected by filtration, and washed with a mixture of ethanol/water (1:1) to obtain 4-(N,N-diphenylamino)benzaldehyde in an amount of 91.5 g (yield: 81.0%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06296978B1uspto-grants-2001_10