Toluene → Zirconium(2+) dicyclopenta-2,4-dien-1-ide

HRID 1977518Notes

Reaction equation

HRID 1977518 reaction equation
[Cl-].[Cl-].[Cl-].[Cl-].[Zr+4:5].[C:6]1([CH3:12])[CH:11]=[CH:10][CH:9]=CC=1>>[CH-:9]1[CH:10]=[CH:11][CH:6]=[CH:12]1.[CH-:9]1[CH:10]=[CH:11][CH:6]=[CH:12]1.[Zr+2:5]

Participants

3

Reactant 2

HCID 1140Toluene2×HCID 9856075Zirconium chloride (ZrCl4), (T-4)-

Product 1

HCID 15183825Zirconium(2+) dicyclopenta-2,4-dien-1-ide

Conditions

Temperature
-30 °C

Procedure

1H NMR (d8-THF): δ 1.4 (d, 12H, Me), 3.22 (s, 4H, bridge CH2), 3.4 (septet, 2H, CHMe2), 5.93 (s, 2H, CH), 6.28 (m, 4H, aromatic CH), 7.08 (t, 2H, aromatic CH), 7.22 (t, 2H, aromatic CH), 7.28 (t, 4H, aromatic CH), 7.66 (d, 4H, aromatic CH) ppm. The dianion was suspended in toluene and cooled to −30° C.; 0.15 g of ZrCl4 (0.64 mmol) were added and the reaction mixture was stirred for 4 hours at 20° C. and then centrifuged. Toluene was discarded and the remaining powder was extracted with CH2Cl2. Centrifugation afforded a mixture of the two isomers rec/meso-1,2-ethylene-bis(1-isopropyl4-phenyl-2-indenyl)zirconium dichloride, about in a 1:1 ratio.

Workup

  1. extractionthe remaining powder was extracted with CH2Cl2
  2. customCentrifugation afforded

Sources & evidence

ORD record
ord-6967d5d083c54392b7595d822d80df46
Source dataset
uspto-grants-2001_05
Patent number
US06232484B1

Reaction notes

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