ChemicalBook CAS DataBase List Bis(cyclopentadienyl)zirconium dichloride

Bis(cyclopentadienyl)zirconium dichloride synthesis

5synthesis methods

Product Name:Bis(cyclopentadienyl)zirconium dichloride
CAS Number:1291-32-3
Molecular formula:C10H10Cl2Zr
Molecular Weight:292.32

Synthesis of zirconium dichlorodichloride
A stirring magnet was placed in a 500 mL three-necked flask, fitted with a constant pressure dropping funnel and reflux condenser, evacuated, and replaced with pure nitrogen three times. The flask was added with 50mL of toluene and 22.3g (0.1mol) of ZrCl4, and the suspension was made by turning on the stirring. Add the THF solution of sodium cyclopentadienylide to a constant pressure dropping funnel, add dropwise at room temperature, keep the reaction solution slightly boiling, after the dropwise addition, continue the reaction for 2h. Under the heating of oil bath at 50℃, evaporate the solvent under reduced pressure to obtain a yellow solid. Put the solid into a soxhlet extractor and extract with CHCl3. Most of the solvent in the extract was evaporated under reduced pressure, and the solid was precipitated after cooling and filtered. The product was washed with a small amount of CHCl3 and dried under vacuum, yielding 20.2g of white crystals, 69% yield.

10026-11-6 Synthesis

10026-11-6
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Bis(cyclopentadienyl)zirconium dichloride

1291-32-3
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$10.00/1g

Yield:1291-32-3 95%

Reaction Conditions:

with n-butyllithium in hexane;byproducts: LiCl; suspn. of ZrCl4 in hexane under Ar cooled to -78°C, treated with BuLi in hexane, warmed to 20°C over 8 h, cooled to -78°C, treated with Cp for 1 h at -78°C, refluxed for 4 h, cooled; filtered, extd. with pentane-CH2Cl2, volatiles were removed under reduced pressure;

References:

Eisch, John J.;Owuor, Fredrick A.;Otieno, Peter O. [Organometallics,2001,vol. 20,# 20,p. 4132 - 4134]