反応 #465941

ord-17534e2ccb6c45a8bd9e00cfe1233de6

反応方程式

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
収率 81.0%

溶媒

反応条件

温度
95°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他reaction for 5 hours
  2. 2
    その他The reaction solution obtained
  3. 3
    workup.STIRRINGby stirring for 1 hour
  4. 4
    その他Thereafter, the precipitate formed
  5. 5
    ろ過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, 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%).

出典

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