反応 #472485

ord-35fc707845934b1e8ddf48bda767520c

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction mixture was purged with nitrogen for 30 min
  2. 2
    温度was heated up
  3. 3
    温度to reflux for overnight under nitrogen
  4. 4
    温度The reaction mixture was cooled
  5. 5
    その他the organic extracts were purified by column chromatography and recrystallization with toluene

実験手順

4.4 g (14.6 mmol) of 2-bromotriphenylene, 4.0 g (17.5 mmol) of 4-dibenzothiopheneboronic acid, 0.51 g (0.44 mmol) of tetrakistriphenylphosphinepalladium, and 4.0 g (43.4 mmol) of potassium carbonate were charged in a 250 mL round bottom flask with solvent 90 mL of toluene and 10 mL of water. The reaction mixture was purged with nitrogen for 30 min and then was heated up to reflux for overnight under nitrogen with stirring. The reaction mixture was cooled and the organic extracts were purified by column chromatography and recrystallization with toluene. 5.1 g (86%) of white solid was obtained as the product which was confirmed by proton NMR.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08367850B2uspto-grants-2013_02