反応 #610220

ord-7ec1e1daec74415eb752c37fb64bac92

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 1 h
  2. 2
    抽出The mixture is then extracted with dichloromethane
  3. 3
    その他The solvent is evaporated in vacuo
  4. 4
    その他the residue is purified by chromatography (heptane/ethyl acetate 10:1)

実験手順

97 g (123 mmol) of 3,3″-bis(phenyl)-9′-[(phenyl)sulfonyl]-9,3′:6′,9″-ter-9H-carbazole and 48 g (856 mmol) of potassium hydroxide in 65 ml of dimethyl sulfoxide and 21 ml of water are heated under reflux for 1 h. The mixture is subsequently cooled to room temperature and neutralised using 1 M HCl solution. The mixture is then extracted with dichloromethane. The solvent is evaporated in vacuo, and the residue is purified by chromatography (heptane/ethyl acetate 10:1). Yield: 64.8 g (100 mmol), 80%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09334260B2uspto-grants-2016_05