Tetrahydrofuran → HCID 178421900, compound

HRID 355552

Reaction equation

HRID 355552 reaction equation
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C[Si:8](C)([CH:19]1[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[C:20]1[CH3:28])C1C2C(=CC=CC=2)C=C1C.[Cl-:30].[Cl-].[Cl-].[Cl-].[Zr+4:34].O1CCC[CH2:36]1>C(Cl)Cl>[Cl-:30].[Cl-:30].[CH3:36][C:3]1[CH:4]=[CH:5][C-:6]([CH:19]2[C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:21]=[C:20]2[CH3:28])[C:2]=1[CH3:1].[SiH2:8]=[Zr+2:34].[CH3:28][C:20]1[CH:19]([C-:2]2[CH:3]=[CH:4][CH:5]=[CH:6]2)[C:27]2[C:22]([CH:21]=1)=[CH:23][CH:24]=[CH:25][CH:26]=2

Participants

6

Reactant 4

HCID 8028TetrahydrofuranHCID 8058HexaneHCID 4050248Dimethyl-bis(2-methyl-1H-inden-1-yl)silaneHCID 9856075Zirconium chloride (ZrCl4), (T-4)-

Product 1

HCID 178421900HCID 178421900, compoundYield 35%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

15.3 ml (38.4 mmol) of a 2.5 molar solution of buthyllithium hexane were added to a solution of 6.07 g (19.2 mmol) dimethylbis(2-methylindenyl)-silane in 80 ml tetrahydrofuran. The mixture was refluxed for 2 hours prior to solvent evaporation. The residue was suspended in 30 ml of hexane, the suspension was filtrated and the dilithio-compound was dried in vacuo. The dilithio-compound was then added to a suspension of 4.47 g (19.2 mmol) zirconiumtetrachloride in 50 ml metylenchloride at -78° C. The suspension was slowly warmed to room temperature and stirred over night. The suspension was filtrated and the meso-compound was removed by extraction with toluene. The residue was extracted with 70 ml methylenchloride, the filtrat was concentrated and stored for crystallisation at -30° C. Filtration of the suspension afforded 3,20 g (35%) rac-dimethylsilandiylbis(2-methylindenyl)zirconocen dichloride.

Workup

  1. temperatureThe mixture was refluxed for 2 hours
  2. customto solvent evaporation
  3. filtrationthe suspension was filtrated
  4. dry with materialthe dilithio-compound was dried in vacuo
  5. filtrationThe suspension was filtrated
  6. customthe meso-compound was removed by extraction with toluene
  7. extractionThe residue was extracted with 70 ml methylenchloride
  8. concentrationthe filtrat was concentrated
  9. customstored for crystallisation at -30° C
  10. filtrationFiltration of the suspension

Sources & evidence

ORD record
ord-b1d0fa4901ef4ca39ca00bbaa9d3809a
Source dataset
uspto-grants-1998_11
Patent number
US05831105

Linked notes

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