Reaktion #468423

Reaktionsgleichung

ZrCl4

toluene

toluene

→

zirconocene

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe above obtained dianion
2. 2
   TemperaturThe reaction mixture was maintained
3. 3
   WaschenThe remaining powder was washed with toluene (20 mL)
4. 4
   Extraktionextracted with CH2Cl2, in order
5. 5
   Sonstigeto separate the product from LiCl
6. 6
   workup.ADDITIONA pure mixture of rac
7. 7
   Sonstigewas obtained, in the form of a yellow powder
8. 8
   SonstigeBy crystallization from toluene
9. 9
   Sonstigethe meso isomer could be completely separated from the rac-isomer
10. 10
    SonstigeThe rac-isomer was obtained as a rac
11. 11
    workup.ADDITIONmixture of about 4:1

Vorschrift

The above obtained dianion was suspended in toluene and cooled to −20° C.; to the obtained mixture were added 0.28 g (1.19 mmol; 1.05 equivalents) of ZrCl4. The reaction mixture was maintained under stirring for 16 hours, at 20° C.; then it was centrifuged and the toluene layer was discarded. The remaining powder was washed with toluene (20 mL) and then extracted with CH2Cl2, in order to separate the product from LiCl. A pure mixture of rac and meso-isomers of 1,2-ethylene-bis(4-phenyl-2-indenyl)zirconium dichloride was obtained, in the form of a yellow powder. By crystallization from toluene, the meso isomer could be completely separated from the rac-isomer. The rac-isomer was obtained as a rac:meso mixture of about 4:1.

Quelle