Zirconium chloride (ZrCl4), (T-4)- → HCID 178440793, compound

HRID 1198308Notes

Reaction equation

HRID 1198308 reaction equation
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2([Li])[CH:15]=[CH:14][CH:13]=[CH:12]2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[Cl-:17].[Cl-].[Cl-].[Cl-].[Zr+4:21]>O1CCCC1.C1(C)C=CC=CC=1.ClCCl>[Cl-:17].[Cl-:17].[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2([Zr+2:21][C:11]3([C:8]4[CH:7]=[CH:6][C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:10][CH:9]=4)[CH:15]=[CH:14][CH:13]=[CH:12]3)[CH:15]=[CH:14][CH:13]=[CH:12]2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]

Participants

6

Reactant 2

HCID 9856075Zirconium chloride (ZrCl4), (T-4)-HCID 178506636HCID 178506636, compound

Product 1

HCID 178440793HCID 178440793, compound

Reagents, catalysts & solvents 3

HCID 1140TolueneSolventHCID 6344DichloromethaneSolventHCID 8028TetrahydrofuranSolvent2×

Procedure

A solution of 1.2 g of 4-t-butylphenylcyclopentadienyllithium (0.0059 mole) in 20 ml tetrahydrofuran was slowly added at room temperature to a solution of 0.685 g of zirconium tetrachloride (0.0029 mole) in 50 ml tetrahydrofuran. After stirring the solution for 2 hours, the tetrahydrofuran was removed by evaporation leaving a residue. The resulting residue was taken up in hot toluene. Any undissolved material was removed by filtration and a resultant clear solution was evaporated to dryness. The solid residue obtained from the evaporation to dryness was taken up in dichloromethane. Undissolved, off-white solids were removed by centrifugation and decantation. The clear solution was once again evaporated to dryness yielding bis[(4-t-butylphenyl)cyclopentadienyl]zirconium dichloride as a yellow solid material. Spectral data from a proton-NMR is consistent with the product obtained.

Workup

  1. customthe tetrahydrofuran was removed by evaporation
  2. customleaving a residue
  3. customAny undissolved material was removed by filtration
  4. customa resultant clear solution was evaporated to dryness
  5. customThe solid residue obtained from the evaporation to dryness
  6. customoff-white solids were removed by centrifugation and decantation
  7. customThe clear solution was once again evaporated to dryness

Sources & evidence

ORD record
ord-3a3990e5968c4647beabb5bf27d39dbe
Source dataset
uspto-grants-1994_01
Patent number
US05279999

Reaction notes

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