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

HRID 1838519Notes

Reaction equation

HRID 1838519 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-e533ace0f8e64f47948211e5647fc759
Source dataset
uspto-grants-2004_01
Patent number
US06673880B2

Reaction notes

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