반응 #468423

반응 방정식

ZrCl4

toluene

toluene

→

zirconocene

반응 조건

후처리

1. 1
   기타The above obtained dianion
2. 2
   온도The reaction mixture was maintained
3. 3
   세척The remaining powder was washed with toluene (20 mL)
4. 4
   추출extracted with CH2Cl2, in order
5. 5
   기타to separate the product from LiCl
6. 6
   workup.ADDITIONA pure mixture of rac
7. 7
   기타was obtained, in the form of a yellow powder
8. 8
   기타By crystallization from toluene
9. 9
   기타the meso isomer could be completely separated from the rac-isomer
10. 10
    기타The rac-isomer was obtained as a rac
11. 11
    workup.ADDITIONmixture of about 4:1

실험 절차

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.

출처