反应详情

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.

1. temperatureThe mixture was refluxed for 2 hours
2. customto solvent evaporation
3. filtrationthe suspension was filtrated
4. dry with materialthe dilithio-compound was dried in vacuo
5. filtrationThe suspension was filtrated
6. customthe meso-compound was removed by extraction with toluene
7. extractionThe residue was extracted with 70 ml methylenchloride
8. concentrationthe filtrat was concentrated
9. customstored for crystallisation at -30° C
10. filtrationFiltration of the suspension