Fluorene → 1,1-Cyclopentadienyl(9-fluorenyl)dipenylmethane

HRID 1376665

Reaktionsgleichung

Reaktionsgleichung von HRID 1376665
[CH3:1]CCCCC.[CH2:7]([Li])[CH2:8][CH2:9][CH3:10].[CH:12]1[C:24]2[CH2:23][C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16]=2[CH:15]=[CH:14][CH:13]=1.[C:25]1([C:31]2[CH:35]=[CH:34][C:33](=[CH2:36])[C:32]=2[C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)C=CC=CC=1>C1COCC1.O>[C:10]1([C:32]([CH:23]2[C:22]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:16]3[C:24]2=[CH:12][CH:13]=[CH:14][CH:15]=3)([C:31]2[CH:25]=[CH:36][CH:33]=[CH:34][CH:35]=2)[C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)[CH2:1][CH2:7][CH2:8][CH:9]=1

Komponenten

7

Edukt 4

HCID 6853FluoreneHCID 8058HexaneHCID 22238549Diphenyl FulveneHCID 178418339Butyllithium

Produkt 1

HCID 227351321,1-Cyclopentadienyl(9-fluorenyl)dipenylmethaneAusbeute 42 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Diphenylenemethylene(9-fluorenyl)(cyclopentadienyl)zirconium dichloride ##STR11## 12.3 cm3 (30.7 mmol) of a 2.5 molar hexane solution of n-butyllithium were slowly added to a solution of 5.10 g (30.7 mmol) of fluorene in 60 cm3 of THF at room temperature. After 40 minutes, 7.07 g (30.7 mmol) of diphenylfulvene were added to the orange solution, and the mixture was stirred overnight. 60 cm3 of water were added to the dark red solution, as a result of which the solution turns yellow, and the solution was extracted with ether. The ether phase was dried over MgSO4, concentrated, and allowed to crystallize at -35° C. 5.1 g (42%) of 1,1-cyclopentadienyl-(9-fluorenyl)diphenylmethane was obtained as a beige powder.

Aufarbeitung

  1. customas a result of which the solution
  2. extractionthe solution was extracted with ether
  3. dry with materialThe ether phase was dried over MgSO4
  4. concentrationconcentrated
  5. customto crystallize at -35° C

Quellen und Nachweise

ORD-Eintrag
ord-2ba957d05f104a3588cc47ed587a0aa0
Quelldatensatz
uspto-grants-1997_09
Patentnummer
US05663268

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