Reaktion #2139924
ord-e3e4ddff55fb4d9fbf83ffd6880dc13d
Reaktionsgleichung
fluorenone
2-bromobiphenyl
→
9.9′-Spirobifluorene
Ausbeute 80.0%
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONwas added
- 2Temperaturrefluxed
- 3FiltrationThe produced yellow precipitate was filtered
- 4workup.STIRRINGstirred in cold ammonium chloride
- 5Filtrationthe obtained crystal was filtered again
- 6Sonstigedried
- 7workup.ADDITIONThereafter, acetic acid was added to the solid product
- 8Temperaturthe solution was refluxed
- 9workup.STIRRINGwhile stirring
- 10workup.ADDITIONA small amount of hydrochloric acid was added
- 11Sonstigeto obtain the solid target compound
- 12FiltrationThe solid target compound was filtered
- 13Waschenwashed
- 14Sonstigeto 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%.