Reaktion #814018

Reaktionsgleichung

hafnium tetrachloride

dilithium

toluene

→

hafnocene dichloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe reaction
2. 2
   FiltrationInsoluble constituents are then filtered off via a frit
3. 3
   Sonstigethe orange-red filtrate is evaporated to dryness on an oil pump
4. 4
   workup.ADDITION30 ml of pentane are added to the orange-red residue
5. 5
   workup.STIRRINGthe mixture is stirred vigorously overnight
6. 6
   SonstigeRemoval of the solvent in vacuo

Vorschrift

1.81 g (5.65 mmol) of hafnium tetrachloride are added to a suspension, cooled to -78° C., of 2.00 g (5.64 mmol) of the dilithium salt (Example 4) in 150 ml of toluene. The orange suspension is allowed to warm to room temperature, and is stirred for a further 2 days in order to complete the reaction. Insoluble constituents are then filtered off via a frit, and the orange-red filtrate is evaporated to dryness on an oil pump. 30 ml of pentane are added to the orange-red residue, and the mixture is stirred vigorously overnight. Removal of the solvent in vacuo gives the hafnocene dichloride as beige powder in a crude product yield of 700 mg (24%). The 1H-NMR spectrum of the crude product shows only one diastereomer.

Quelle