反应详情

A solution of 67.8 mmol of lithium-fluorene in 50 cm3 of tetrahydrofuran was added to a solution of 11.4 g (67.8 mmol) of 6-methyl-6-phenylfulvene in 40 cm3 of tetrahydrofuran at room temperature. After the mixture had been stirred at room temperature for 2 hours, 60 cm3 of water were added. The substance which precipitated out was filtered off with suction, washed with diethyl ether and dried under an oil pump vacuum. 19.2 g (84.2%) of 1-cyclopentadienyl-1-(9-fluorenyl)-ethylbenzene were obtained (correct elemental analyses; 1 H-NMR spectrum). 10.0 g (19.9 mmol) of the compound were dissolved in 60 cm3 of tetrahydrofuran and 26 cm3 (65 mmol) of a 2.5 molar hexane solution of n-butyllithium were added at 0° C. After the mixture had been stirred for 15 minutes, the solvent was stripped off in vacuo. The dark red residue which remained was washed several times with hexane and dried under an oil pump vacuum. 15.6 g of the red dilithium salt were obtained as the tetrahydrofuran adduct which contained about 30% of tetrahydrofuran. A suspension of 4.78 g (14.9 mmol) of HfCl4 in 70 cm3 of CH2CH2 was reacted with 14.9 mmol of the dilithium salt and the reaction product was worked up. Crystallization at -35° C. gave 2.6 g (30%) of the hafnocene dichloride compound as orange crystals. Correct elemental analysis.

1. customThe substance which precipitated out
2. filtrationwas filtered off with suction
3. washwashed with diethyl ether
4. customdried under an oil pump vacuum