Zirconocene dichioride → Bis(5-methylcyclopenta-1,3-diene);zirconium(2+)

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Reaction Steps

Following the literature procedure [b], 3.30 ml (5.33 mmol, 1.60M) of an ethereal solution of methyllithium are slowly added dropwise at -78° C. to a suspension of 1.03 g (2.66 mmol) of zirconocene dichloride (Example 10) in 50 ml of diethyl ether. The mixture is allowed to warm slowly to room temperature in a cold bath and is then stirred at room temperature for a further 5 hours. The solvent is removed in vacuo, and the colorless residue is extracted with 3×50 ml of pentane. The combined pentane solutions are evaporated and kept at -2° C. to crystallize. Removal of the solvent and drying in an oil-pump vacuum gives 700 mg (76%) of dimethylzirconocene as a colorless, crystalline powder.

Provenance & Evidence