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

HRID 1603979Notes

Reaction equation

HRID 1603979 reaction equation
Cl.Cl.Cl.Cl.[Zr:5].[CH3:6][CH2:7][CH2:8][CH2:9][CH3:10]>C1(C)C=CC=CC=1>[CH-:8]1[CH:9]=[CH:10][CH:6]=[CH:7]1.[CH-:8]1[CH:9]=[CH:10][CH:6]=[CH:7]1.[Zr+2:5]

Participants

4

Reactant 2

HCID 8003PentaneHCID 131720402Zirconium tetrahydrochloride

Product 1

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

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

1.58 g (6.79 mmol) of zirconium tetrahydrochloride are added in portions to a suspension, cooled to -78° C., of 2.60 g (6.79 mmol) of the bistrimethylsilyl-substituted dilithium salt in 100 ml of toluene. The mixture is allowed to warm to room temperature, giving, after stirring for 24 hours, an orange suspension. Insoluble constituents are separated off, and the solvent is evaporated to dryness, giving a red oil. Addition of 20 ml of pentane followed by work-up gives the two diastereomers of the ansa-zirconocene as an orange powder in a crude yield of 1.54 g (43%); m.p. 151° C. (decomp., DSC).

Workup

  1. customgiving
  2. customInsoluble constituents are separated off
  3. customthe solvent is evaporated to dryness
  4. customgiving a red oil

Sources & evidence

ORD record
ord-5d132954e79d46539a12f4f9b4c8c9f7
Source dataset
uspto-grants-1999_11
Patent number
US05990254

Reaction notes

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