2-Bromobiphenyl → 9,9'-Spirobi(9H-fluorene)

HRID 2052742

Reaktionsgleichung

Reaktionsgleichung von HRID 2052742
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[C:14]1(=O)[C:26]2[C:18]([C:19]3[C:24]([CH:25]=2)=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:17][CH:16]=[CH:15]1>CCOCC>[CH:7]1[C:2]2[C:25]3([C:26]4[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=4[C:19]4[C:24]3=[CH:23][CH:22]=[CH:21][CH:20]=4)[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:3]=2[CH:4]=[CH:5][CH:6]=1

Komponenten

4

Edukt 2

HCID 163292-BromobiphenylHCID 22281833Fluoreneone

Produkt 1

HCID 1359759,9'-Spirobi(9H-fluorene)Ausbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

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%.

Aufarbeitung

  1. additionwas added
  2. temperaturerefluxed
  3. filtrationThe produced yellow precipitate was filtered
  4. stirringstirred in cold ammonium chloride
  5. filtrationthe obtained crystal was filtered again
  6. customdried
  7. additionThereafter, acetic acid was added to the solid product
  8. temperaturethe solution was refluxed
  9. stirringwhile stirring
  10. additionA small amount of hydrochloric acid was added
  11. customto obtain the solid target compound
  12. filtrationThe solid target compound was filtered
  13. washwashed
  14. customto obtain pure target compound with the yield of 80%

Quellen und Nachweise

ORD-Eintrag
ord-e3e4ddff55fb4d9fbf83ffd6880dc13d
Quelldatensatz
uspto-grants-2008_02
Patentnummer
US07326474B2

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