反応 #465948

ord-11207b0ea3704e8ba58a1b40706a1ef4

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was heated
  2. 2
    温度refluxed
  3. 3
    ろ過the reaction solution was filtered
  4. 4
    洗浄The filtrate was successively washed with an aqueous 3 to 5% sodium thiosulfate solution and saturated brine
  5. 5
    乾燥The organic layer was dried with anhydrous sodium sulfate
  6. 6
    その他the solvent was removed
  7. 7
    その他The resulting crude reaction product
  8. 8
    その他was recrystallized from ethanol

実験手順

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%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06296978B1uspto-grants-2001_10