تفاعل #465941

ord-17534e2ccb6c45a8bd9e00cfe1233de6

معادلة التفاعل

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
المردود 81.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
95°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىreaction for 5 hours
  2. 2
    أخرىThe reaction solution obtained
  3. 3
    workup.STIRRINGby stirring for 1 hour
  4. 4
    أخرىThereafter, the precipitate formed
  5. 5
    ترشيحwas collected by filtration
  6. 6
    غسيلwashed with a mixture of ethanol/water (1:1)

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06296978B1uspto-grants-2001_10