Reaktion #442734

Reaktionsgleichung

zirconiumtetrachloride

hexane

dimethylbis(2-methylindenyl)-silane

tetrahydrofuran

→

rac-dimethylsilandiylbis(2-methylindenyl)zirconocen dichloride

Ausbeute 35.0%

Lösungsmittel

metylenchloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was refluxed for 2 hours
2. 2
   Sonstigeto solvent evaporation
3. 3
   Filtrationthe suspension was filtrated
4. 4
   Trocknenthe dilithio-compound was dried in vacuo
5. 5
   FiltrationThe suspension was filtrated
6. 6
   Sonstigethe meso-compound was removed by extraction with toluene
7. 7
   ExtraktionThe residue was extracted with 70 ml methylenchloride
8. 8
   Einengenthe filtrat was concentrated
9. 9
   Sonstigestored for crystallisation at -30° C
10. 10
    FiltrationFiltration of the suspension

Vorschrift

15.3 ml (38.4 mmol) of a 2.5 molar solution of buthyllithium hexane were added to a solution of 6.07 g (19.2 mmol) dimethylbis(2-methylindenyl)-silane in 80 ml tetrahydrofuran. The mixture was refluxed for 2 hours prior to solvent evaporation. The residue was suspended in 30 ml of hexane, the suspension was filtrated and the dilithio-compound was dried in vacuo. The dilithio-compound was then added to a suspension of 4.47 g (19.2 mmol) zirconiumtetrachloride in 50 ml metylenchloride at -78° C. The suspension was slowly warmed to room temperature and stirred over night. The suspension was filtrated and the meso-compound was removed by extraction with toluene. The residue was extracted with 70 ml methylenchloride, the filtrat was concentrated and stored for crystallisation at -30° C. Filtration of the suspension afforded 3,20 g (35%) rac-dimethylsilandiylbis(2-methylindenyl)zirconocen dichloride.

Quelle