Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pentane | HCID 8003 | — |
| Reactant | Tributyltin fluoride | HCID 16120 | — |
| Reactant | HCID 178440521 | HCID 178440521 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178440522 | HCID 178440522 | — |
Reaction Steps
To a straw yellow solution of bis(propylcyclopentadienyl) zirconium dichloride [(PrCp)2ZrCl2] (1.00 g, 2.66 mmol, 1.00 eq.) in dichloromethane (10 mL) was added tributyltin fluoride (1.72 g, 5.57 mmol, 2.10 eq.). The reaction rapidly lightened, turning almost colorless. The reaction was stirred 1 h and was then filtered to give a colorless solution and a small amount of white solid. The solution was evaporated in vacuo, leaving a damp, white solid. Pentane (10 mL) was added and the mixture was cooled to −35° C. The mixture was filtered, and resulting white solid was washed with pentane (3×3 mL) cooled to −35° C. The white solid was dried in vacuo to yield 0.75 g (82%). 1H NMR(CD2Cl2): δ0.92 (t, 6H, CH2CH2CH3), 1.56 (m, 4H, CH2CH2CH3), 2.44 (t, 4H, CH2CH2CH3), 6.05 (m, 4H, ring-H), 6.30 (m, 4H, ring-H). 19F NMR(CD2Cl2): δ20.4 (s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06632901B2 |
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| Source dataset | uspto-grants-2003_10 |
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| ORD ID | ord-47db7a86b0bf4b8abbe9af4e306d5a0a |
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| Source note | uspto-grants-2003_10 |
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