反応 #70660

ord-cc59a0d0fd4b424daff87e80c3c72591

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the solvent was removed by evaporation
  2. 2
    workup.ADDITION1000 mL Ethyl acetate was added
  3. 3
    抽出the reaction mixture was extracted
  4. 4
    乾燥The combined organic layer was dried over magnesium sulfate
  5. 5
    ろ過After filtration
  6. 6
    その他the solvent was removed by evaporation

実験手順

To a three-neck round-bottom flask, were added 34.0 g N2,N7-bis(3-(1,3-dioxolan-2-yl)phenyl)-9,9-dioctyl-N2,N7-di-m-tolyl-9H-fluorene-2,7-diamine and in 1000 mL acetone. 189.5 mL 2 M hydrochloric acid solution was added slowly to the reaction mixture through an addition funnel. The reaction was monitored by TLC. After the reaction was done showed by TLC, the solvent was removed by evaporation. 1000 mL Ethyl acetate was added, and the reaction mixture was extracted using DI water (3×750 mL). The combined organic layer was dried over magnesium sulfate. After filtration, the solvent was removed by evaporation. The product (27.8 g) was obtained, and was carried on to next reaction without further purification. The structure was confirmed by NMR.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08535974B2uspto-grants-2013_09