Toluene → Zirconium(2+) dicyclopenta-2,4-dien-1-ide

Temperature

-20 °C

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.

1. customThe above obtained dianion
2. temperatureThe reaction mixture was maintained
3. washThe remaining powder was washed with toluene (20 mL)
4. extractionextracted with CH2Cl2, in order
5. customto separate the product from LiCl
6. additionA pure mixture of rac
7. customwas obtained, in the form of a yellow powder
8. customBy crystallization from toluene
9. customthe meso isomer could be completely separated from the rac-isomer
10. customThe rac-isomer was obtained as a rac
11. additionmixture of about 4:1

ORD record

ord-e197a32891f74599a5e2f86aef1eda16

Source dataset

uspto-grants-2001_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06232484B1