反应详情

12.3 cm3 (30.7 mmol) of a 2.5 molar hexane solution of n-butyllithium were slowly added to a solution of 5.10 g (30.7 mmol) of fluorene in 60 cm3 of tetrahydrofuran at room temperature. After 40 minutes, 7.07 g (30.7 mmol) of diphenylfulvene were added to the orange solution and the mixture was stirred overnight. 60 cm3 of water were added to the dark red solution, whereupon the solution became yellow-colored, and the mixture was extracted with ether. The ether phase was dried over MgSO4 and concentrated and the residue was left to crystallize at -35° C. 5.1 g (42%) of 1-cyclopentadienyl-1-(9-fluorenyl)-diphenylmethane were obtained as a beige powder. 1.25 g (3.15 mmol) of 1-cyclopentadienyl-1-(9-fluorenyl)-diphenylmethane were reacted with 6.3 mmol of butyllithium analogously to Example 1. The dilithium salt was reacted with 1.0 g (3.15 mmol) of HfCl4 analogously to Example 1. Filtration of the orange reaction mixture over a G4 frit and extraction of the filtrate with 100 cm3 of toluene gave 0.70 g (34%) of the hafnocene dichloride complex as a yellow-orange powder. Correct elemental analysis. The mass spectrum gave M+ =644.

1. extractionthe mixture was extracted with ether
2. dry with materialThe ether phase was dried over MgSO4
3. concentrationconcentrated
4. waitthe residue was left
5. customto crystallize at -35° C