반응 #465948

ord-11207b0ea3704e8ba58a1b40706a1ef4

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    온도refluxed
  3. 3
    여과the reaction solution was filtered
  4. 4
    세척The filtrate was successively washed with an aqueous 3 to 5% sodium thiosulfate solution and saturated brine
  5. 5
    건조The organic layer was dried with anhydrous sodium sulfate
  6. 6
    기타the solvent was removed
  7. 7
    기타The resulting crude reaction product
  8. 8
    기타was recrystallized from ethanol

실험 절차

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%).

출처

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