반응 #465941

ord-17534e2ccb6c45a8bd9e00cfe1233de6

반응 방정식

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
수율 81.0%

용매

반응 조건

온도
95°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06296978B1uspto-grants-2001_10