Reaktion #1768625

ord-20f1cf1f102d436490a6f219f35078e1

Lösungsmittel

Reaktionsbedingungen

Temperatur
-20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeIn a nitrogen-purged Schlenk reaction vessel
  2. 2
    Sonstigewas gradually brought to room temperature
  3. 3
    workup.STIRRINGstirred continuously for 2 days
  4. 4
    Filtrationthe formed precipitate was collected by filtration
  5. 5
    Sonstigedried
  6. 6
    Sonstigerecrystallized

Vorschrift

In a nitrogen-purged Schlenk reaction vessel, 97.4 mg (0.37 mmol) of dichloromethylenebis(cyclopentadienyl)titanium was weighted out. Thereto 20 ml of dried toluene was added, and the mixture was cooled to -20° C. A solution of 1.4 mmol of methylalumoxane (tetramer) in benzene was added thereto dropwise with stirring over one hour. The reaction solution was gradually brought to room temperature, and then stirred continuously for 2 days. The reaction solution changed gradually its color from violet to reddish brown. Hexane was added thereto, and the formed precipitate was collected by filtration, dried and recrystallized. The yield was 82%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05171871uspto-grants-1992_12