Zirconium chloride (ZrCl4), (T-4)- → HCID 178440525, compound

Temperature

20 °C

A solution of 0.105 mol of methyllithium in ether is added slowly to a solution, vigorously stirred at 0° C., of the β-propenylcyclopentadiene prepared in the preceding stage (a) in ether. The mixture is heated to ambient temperature (20° C.) and is kept stirred for 1 hours. A precipitate of β-propenylcyclopentadienyllithium is isolated by filtration, washed with ether 2′ 100 ml) and dried to give a white powder. 47.5 millimoles of zirconium tetrachloride dissolved in 100 ml of THF are added to a vigorously stirred solution of β-propenylcyclopentadienyllithium in 100 ml of THF at 0° C. The mixture is heated to ambient temperature (20° C.) and is stirred for 16 hours. The volatile compounds are removed under vacuum and the residue is extracted with ether (4′ 100 ml) and filtered. The product is obtained in the form of a white solid by slow cooling of the solution to −78° C. and recrystallization from cold ether.

1. washwashed with ether 2′ 100 ml) and
2. customdried
3. customto give a white powder
4. customThe volatile compounds are removed under vacuum
5. extractionthe residue is extracted with ether (4′ 100 ml) and
6. filtrationfiltered
7. customThe product is obtained in the form of a white solid
8. temperatureby slow cooling of the solution to −78° C.
9. customrecrystallization from cold ether

ORD record

ord-b42b3fc106a547d18332c5bbb774a01d

Source dataset

uspto-grants-2001_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06174972B1