Toluene → Zirconocene dichioride

HRID 865320Notes

Reaction equation

HRID 865320 reaction equation
[Li][Li].[Cl-:3].[Cl-].[Cl-].[Cl-].[Zr+4:7].[C:8]1([CH3:14])[CH:13]=[CH:12][CH:11]=CC=1>>[Cl-:3].[Cl-:3].[CH-:11]1[CH:12]=[CH:13][CH:8]=[CH:14]1.[CH-:11]1[CH:12]=[CH:13][CH:8]=[CH:14]1.[Zr+2:7]

Participants

4

Reactant 3

HCID 1140TolueneHCID 139759Lithium, mol. (Li2)HCID 9856075Zirconium chloride (ZrCl4), (T-4)-

Product 1

HCID 131716798Zirconocene dichioride

Conditions

Temperature
-78 °C

Procedure

A suspension of 7.80 g (22.0 mmol) of the dilithium salt (EXAMPLE 4) in 200 ml of toluene is cooled to -78° C., and 5.10 g (22.0 mmol) of zirconium tetrachloride are added in portions. The mixture is allowed to warm to room temperature, and the yellow-orange suspension is stirred for a further 48 hours. Insoluble constituents are filtered off via a frit, and the solvent is removed in an oil-pump vacuum. The red-orange oil is powdered by vigorous stirring with pentane, giving the zirconocene dichioride in a crude yield of 30% (2.72 g).

Workup

  1. temperatureto warm to room temperature
  2. filtrationInsoluble constituents are filtered off via a frit
  3. customthe solvent is removed in an oil-pump vacuum
  4. stirringby vigorous stirring with pentane

Sources & evidence

ORD record
ord-72d7c25387464cd8b214e820caa6b15a
Source dataset
uspto-grants-1996_10
Patent number
US05565534

Reaction notes

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