تفاعل #465948

ord-11207b0ea3704e8ba58a1b40706a1ef4

معادلة التفاعل

c1ccc(Nc2ccccc2)cc1
diphenylamine
Cc1ccc(I)cc1
p-iodotoluene
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
Cc1ccc(N(c2ccccc2)c2ccccc2)cc1
4-methyltriphenylamine
المردود 81.4%

الكواشف

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةrefluxed
  3. 3
    ترشيحthe reaction solution was filtered
  4. 4
    غسيلThe filtrate was successively washed with an aqueous 3 to 5% sodium thiosulfate solution and saturated brine
  5. 5
    تجفيفThe organic layer was dried with anhydrous sodium sulfate
  6. 6
    أخرىthe solvent was removed
  7. 7
    أخرىThe resulting crude reaction product
  8. 8
    أخرىwas recrystallized from ethanol

الإجراء التجريبي

To 30 ml of o-dichlorobenzene, 4.5 g (27 mmol) of diphenylamine, 11.0 g (51 mmol) of p-iodotoluene, 5.5 g (40 mmol) of anhydrous sodium carbonate and 1.1 g of copper powder were added. The mixture was heated and refluxed with stirring for 7 hours. After the reaction was completed, the reaction solution was filtered. The filtrate was successively washed with an aqueous 3 to 5% sodium thiosulfate solution and saturated brine. The organic layer was dried with anhydrous sodium sulfate, and thereafter the solvent was removed. The resulting crude reaction product was recrystallized from ethanol to obtain 4-methyltriphenylamine in an amount of 5.7 g (yield: 81.4%).

المصدر

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