Реакция #465941

ord-17534e2ccb6c45a8bd9e00cfe1233de6

Реагенты

Нет

Растворители

Условия реакции

Температура
95°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06296978B1uspto-grants-2001_10