Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fluorene | HCID 6853 | — |
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Reactant | HCID 178435158 | HCID 178435158 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 178435159 | HCID 178435159 | — |
Reaction Steps
About 2.4 mmol of fluorene was dissolved in 50 ml of diethylether and mixed with 1.5 ml of a 1.6M hexane solution of butyllithium and stirred for 2 hrs at room temperature. Then 0.77 g of bis(methylcyclopentadienyl) zirconium dichloride was added. The reaction mixture was then stirred for an addition 90 mins. Then the solvent was removed using a vacuum. The residue was extracted with toluene and a suspension filtered over sodium sulfate. The filtrate was freed from solvent and taken up in 50 ml of diethylether. Crystallization at -30° C. yields the product bis(methylcyclopentadienyl) (fluorenyl) zirconium chloride, referred to hereinafter as Catalyst No. 79. The x-ray analysis of the solid Catalyst No. 79 is believed to demonstrate that the fluorenyl is a σ-bound ligand rather than a π-bound ligand.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05627247 |
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| Source dataset | uspto-grants-1997_05 |
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| ORD ID | ord-7bfdf0d1f7754999881850028918d657 |
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| Source note | uspto-grants-1997_05 |
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