HCID 178426006, compound → HCID 178427811, compound

HRID 2182631Notes

Reaction equation

HRID 2182631 reaction equation
[Cl-:1].[Cl-].[Cl-].[CH3:4][C:5]1[C:9]([Zr+3:11])([CH3:10])[C:8]([CH3:12])=[C:7]([CH3:13])[C:6]=1[CH3:14].[CH3:15][C:16]1[C:17]([CH3:24])=[C:18]([CH3:23])[C:19]([Li])([CH3:21])[CH:20]=1>O1CCCC1>[Cl-:1].[Cl-:1].[CH3:4][C:5]1[C:9]([Zr+2:11][C:19]2([CH3:21])[CH:20]=[C:16]([CH3:15])[C:17]([CH3:24])=[C:18]2[CH3:23])([CH3:10])[C:8]([CH3:12])=[C:7]([CH3:13])[C:6]=1[CH3:14]

Participants

4

Reactant 2

HCID 178426006HCID 178426006, compoundHCID 178506703HCID 178506703, compound

Product 1

HCID 178427811HCID 178427811, compoundYield 82.5%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

10.0 g (33.6 mmols) of (pentamethylcyclopentadienyl)zirconium trichloride, and 150 ml of tetrahydrofuran were put into a 300-ml two-neck egg-plant flask. To this, dropwise added was a tetrahydrofuran solution (50 ml) of 4.3 g (33.6 mmols) of (tetramethylcyclopentadienyl) lithium that had been separately prepared at 0° C. This was warmed up to room temperature, and then stirred as such for 8 hours. The solvent was evaporated away, and the residue was extracted in 100 ml of dichloromethane. The resulting extract was concentrated and cooled to −20° C. to obtain 5.8 g of (pentamethylcyclopentadienyl)(tetramethylcyclopentadienyl)zirconium dichloride. A part of this was collected and dissolved in dewatered toluene to prepare a catalyst solution having a concentration of 10 μmols/ml.

Workup

  1. additionTo this, dropwise added
  2. customhad been separately prepared at 0° C
  3. customThe solvent was evaporated away
  4. extractionthe residue was extracted in 100 ml of dichloromethane
  5. extractionThe resulting extract
  6. concentrationwas concentrated
  7. temperaturecooled to −20° C.

Sources & evidence

ORD record
ord-e07aad3192f1496a8bb87b1e0d9634c0
Source dataset
uspto-grants-2005_05
Patent number
US06897261B1

Reaction notes

Loading…