반응 #442734

반응 방정식

zirconiumtetrachloride

hexane

dimethylbis(2-methylindenyl)-silane

tetrahydrofuran

→

rac-dimethylsilandiylbis(2-methylindenyl)zirconocen dichloride

수율 35.0%

용매

metylenchloride

반응 조건

후처리

1. 1
   온도The mixture was refluxed for 2 hours
2. 2
   기타to solvent evaporation
3. 3
   여과the suspension was filtrated
4. 4
   건조the dilithio-compound was dried in vacuo
5. 5
   여과The suspension was filtrated
6. 6
   기타the meso-compound was removed by extraction with toluene
7. 7
   추출The residue was extracted with 70 ml methylenchloride
8. 8
   농축the filtrat was concentrated
9. 9
   기타stored for crystallisation at -30° C
10. 10
    여과Filtration of the suspension

실험 절차

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.

출처