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

HRID 381242Notes

Reaction equation

HRID 381242 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 niixture 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-isopropyl-4-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-e0a2b81579b5495ba5ae92607d42549a
Source dataset
uspto-grants-2001_10
Patent number
US06306791B2

Reaction notes

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