反応 #712383

ord-3566772c81b248108aee9b01d8c2853f

反応条件

温度
170°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated
  2. 2
    温度The mixture was cooled to 90° C.
  3. 3
    workup.DISSOLUTIONdissolved
  4. 4
    その他After removing the insolubles
  5. 5
    ろ過by filtration
  6. 6
    濃縮the filtrate was concentrated under reduced pressure
  7. 7
    その他crystallized from methanol (50 ml)

実験手順

9-Phenyl-9H,9′H-[3,3′]bicarbazolyl (12.9 g), 4-bromo-iodobenzene (13.4 g), a copper powder (0.64 g), potassium carbonate (8.34 g), sodium bisulfite (0.49 g), and orthodichlorobenzene (50 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 170° C. for 19.5 hours. The mixture was cooled to 90° C., and dissolved after adding toluene (200 ml). After removing the insolubles by filtration, the filtrate was concentrated under reduced pressure, and crystallized from methanol (50 ml) to obtain a white powder of 9-(4-bromophenyl)-9′-phenyl-9H,9′H-[3,3′]bicarbazolyl (17.30 g; yield 97%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09306175B2uspto-grants-2016_04