HRID2182631

反应详情

EQUATION

反应方程式

HRID 2182631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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

后处理

  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.