反应详情

5.8 ml (5.8 mmol) of a diethyl ether solution of methyllithium were added dropwise under ice cooling under nitrogen to a THF (20 ml) solution including 1.0 g (2.36 mmol) of 1-cyclopentadienyl-1-(2,7-di-tert-butylfluorenyl)cyclohexane synthesized in the above-mentioned (2), followed by stirring at room temperature for 7 hours. Next, the THF was distilled off under nitrogen, and the resultant solid was washed with hexane and then dissolved in dichloromethane cooled to −78° C. To this solution, zirconium tetrachloride 2THF complex (0.81 g, 2.15 mmol) dissolved in dichloromethane was added at −78° C., and after stirring for 24, the temperature of the solution was slowly returned to room temperature.

1. distillationNext, the THF was distilled off under nitrogen
2. washthe resultant solid was washed with hexane
3. dissolutiondissolved in dichloromethane
4. temperaturecooled to −78° C
5. additionwas added at −78° C.
6. stirringafter stirring for 24
7. customwas slowly returned to room temperature