Toluene → HCID 178504314, compound

HRID 1348541Notes

Reaction equation

HRID 1348541 reaction equation
[Cl-:1].[Cl-].[Cl-].[CH:4]1([Zr+3:9])[CH:8]=[CH:7][CH:6]=[CH:5]1.[CH3:10][Si:11]([CH3:22])([CH3:21])[O:12][CH2:13][CH2:14][CH2:15][C-]1C=CC=C1.[K+].[C:24]1([CH3:30])[CH:29]=[CH:28][CH:27]=CC=1>>[Cl-:1].[Cl-:1].[CH:28]1([C:5]2[C:4]([Zr+2:9])([CH2:15][CH2:14][CH2:13][O:12][Si:11]([CH3:21])([CH3:10])[CH3:22])[CH:8]=[CH:7][CH:6]=2)[CH:27]=[CH:30][CH:24]=[CH:29]1

Participants

4

Reactant 3

HCID 1140Toluene2×HCID 86199143Potassium (3-trimethylsiloxypropyl)-cyclopentadienideHCID 178478629HCID 178478629, compound

Product 1

HCID 178504314HCID 178504314, compound

Procedure

To a suspension of 2.46 g (7 mmol) of cyclopentadienyl zirconium trichloride in toluene, a suspension of 1.6 g (7 mmol) of potassium (3-trimethylsiloxypropyl)-cyclopentadienide in toluene is added. A yellow-brown-coloured suspension immediately precipitates. The reaction is maintained for 12 hours. Subsequently, the solution is filtered and concentrated and a crystalline white solid is formed (0.8 g, 2 mmol, 28%). 1H-NMR (C6D6): 5.87 (t, 2H), 5.65 (t, 2H), 3.46 (m, 2H), 2.74 (m, 2H), 1.73 (m, 2H), 0.14 (s, 9H). 13C-NMR (C6D6): 11.6.9, 115.0, 114.7, 112.2, 61.8, 33.6, 26.8, −0.393. Mass spectrum: M+-65(356): 30%.

Workup

  1. additionis added
  2. customA yellow-brown-coloured suspension immediately precipitates
  3. temperatureThe reaction is maintained for 12 hours
  4. filtrationSubsequently, the solution is filtered
  5. concentrationconcentrated
  6. customa crystalline white solid is formed (0.8 g, 2 mmol, 28%)

Sources & evidence

ORD record
ord-8e88224176db4acfa0df229b50d9cf2d
Source dataset
uspto-grants-2007_05
Patent number
US07211538B2

Reaction notes

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