Reaktion #2139924

ord-e3e4ddff55fb4d9fbf83ffd6880dc13d

Reaktionsgleichung

O=C1C=CC=C2C1=Cc1ccccc12
fluorenone
Brc1ccccc1-c1ccccc1
2-bromobiphenyl
c1ccc2c(c1)-c1ccccc1C21c2ccccc2-c2ccccc21
9.9′-Spirobifluorene
Ausbeute 80.0%

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    Temperaturrefluxed
  3. 3
    FiltrationThe produced yellow precipitate was filtered
  4. 4
    workup.STIRRINGstirred in cold ammonium chloride
  5. 5
    Filtrationthe obtained crystal was filtered again
  6. 6
    Sonstigedried
  7. 7
    workup.ADDITIONThereafter, acetic acid was added to the solid product
  8. 8
    Temperaturthe solution was refluxed
  9. 9
    workup.STIRRINGwhile stirring
  10. 10
    workup.ADDITIONA small amount of hydrochloric acid was added
  11. 11
    Sonstigeto obtain the solid target compound
  12. 12
    FiltrationThe solid target compound was filtered
  13. 13
    Waschenwashed
  14. 14
    Sonstigeto obtain pure target compound with the yield of 80%

Vorschrift

As shown in the following reaction 1, 6.1 g of 2-bromobiphenyl and 0.585 g of dried Mg were dissolved with ether, and 4.2 g of fluorenone dissolved in ether was added thereto, and refluxed while stirring overnight. The produced yellow precipitate was filtered, and stirred in cold ammonium chloride, and then the obtained crystal was filtered again and dried. Thereafter, acetic acid was added to the solid product, and the solution was refluxed while stirring. A small amount of hydrochloric acid was added thereto to obtain the solid target compound. The solid target compound was filtered and washed to obtain pure target compound with the yield of 80%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07326474B2uspto-grants-2008_02