Reaktion #1768626

ord-f612cfcda29346c0a8063102342b71a7

Lösungsmittel

Reaktionsbedingungen

Temperatur
-78°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto react at 50° C. for 6 hours
  2. 2
    FiltrationThe solid was collected by filtration
  3. 3
    Sonstigerecrystallized from toluene/hexane
  4. 4
    Sonstigedried
  5. 5
    SonstigeThe intended product was obtained in a yield of 71%

Vorschrift

97.2 mg (0.372 mmol) of dichloromethylenebis(cyclopentadienyl)titanium was weighed out. Thereto 20 ml of dry toluene was added, and the mixture was cooled to a temperature of -78° C. 2.98 mmol of methylalumoxane (16-mer ) in toluene was added thereto dropwise with stirring, and the mixture was allowed to react at 50° C. for 6 hours. Then 20 ml of hexane was added to deposit a reddish brown solid. The solid was collected by filtration, recrystallized from toluene/hexane, and dried. The intended product was obtained in a yield of 71%.

Quelle

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