反応 #721738

ord-1c4d639f2e6c4048a520ae65408c2072

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture is heated
  2. 2
    温度under reflux for 5 h
  3. 3
    温度After cooling
  4. 4
    ろ過the precipitated solid is filtered off with suction
  5. 5
    洗浄washed with water and ethanol
  6. 6
    その他dried
  7. 7
    抽出The residue is extracted with hot toluene
  8. 8
    その他recrystallised from toluene

実験手順

24.10 g (97.92 mmol) of 3-bromo-9H-carbazole 22, 30.93 g (107.71 mmol) of compound 25 and 11.56 g of sodium carbonate are suspended in 2500 ml of dioxane, 2500 ml of toluene and 1000 ml of water. 5.79 g (5.01 mmol) of Pd(PPh3)4 are added to this suspension. The reaction mixture is heated under reflux for 5 h. After cooling, the precipitated solid is filtered off with suction, washed with water and ethanol and dried. The residue is extracted with hot toluene and recrystallised from toluene. The yield is 22.0 g (55%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09324954B2uspto-grants-2016_04