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

HRID 726839Notes

Reaction equation

HRID 726839 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-d6aa5fd0e8b549ec8fc5301fb5aee5dd
Source dataset
uspto-grants-1998_01
Patent number
US05710297

Reaction notes

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