Reaktion #6335

Reaktionsgleichung

zirconium tetrachloride

cumene

aluminium chloride

aluminium

→

zirconocene dichloride

Ausbeute 118.6%

Lösungsmittel

hydrochloric acid

dichloromethane

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture is heated
2. 2
   Temperaturcooled to 25° C.
3. 3
   Sonstigethe two phases are separated
4. 4
   workup.ADDITIONThe lower dichloromethane phase containing zirconocene dichloride
5. 5
   Einengenis concentrated by rotary evaporation
6. 6
   Sonstigethe residual solid is dried under a high vacuum

Vorschrift

17.5 g (0.075 mol) of zirconium tetrachloride are added at 60° C. under nitrogen over 30 minutes to a stirred mixture of 129.7 g (1.265 mol) of cumene, 27.9 g (0.15 mol) of ferrocene, 26.6 g (0.199 mol) of aluminium chloride and 0.7 g (0.025 mol) of aluminium powder. The reaction mixture is heated and then stirred for 1.5 hours at 110° C., cooled to 25° C., and then slowly poured into a cold mixture of -10° C. of 200 ml of dichloromethane and 50 ml of 32% hydrochloric acid. The mixture is then diluted with a further 200 ml of 5% hydrochloric acid under nitrogen and the two phases are separated. The lower dichloromethane phase containing zirconocene dichloride is concentrated by rotary evaporation and the residual solid is dried under a high vacuum, affording 13 g of zirconocene dichloride [59.4% of theory, sublimed 50.5%, m.p. 195° C. (dec.)].

Quelle