تفاعل #465943

ord-694eee9d0e7a4157bdeed6c3d21fc6bc

معادلة التفاعل

Cc1ccc(N(c2ccccc2)c2ccc(C)c(C)c2)cc1C
[N,N-bis(3,4-dimethylphenyl)amino]benzene
CN(C)C=O
DMF
O=P(Cl)(Cl)Cl
phosphorus oxychloride
Cc1ccc(N(c2ccc(C=O)cc2)c2ccc(C)c(C)c2)cc1C
4-[N,N-bis(3,4-dimethylphenyl)amino]benzaldehyde
المردود 79.0%

المذيبات

ظروف التفاعل

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

المعالجة

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

الإجراء التجريبي

Into a three-necked flask, 124.6 g of [N,N-bis(3,4-dimethylphenyl)amino]benzene and 35.5 ml of DMF were placed, and 84.4 ml of phosphorus oxychloride was added dropwise thereto with stirring while cooling with ice water. After the addition was completed, the mixture solution was heated 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 was collected by filtration, and washed with a mixture of ethanol/water (1:1) to obtain 4-[N,N-bis(3,4-dimethylphenyl)amino]benzaldehyde in an amount of 107.6 g (yield: 79.0%).

المصدر

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