反应详情

The cyclopentadienyl-type ligand, (fluorenyl)(cyclopentadienyl)(methyl)methane was prepared as follows. A solution of 5.0 g fluorene (0.030 mole) was treated with 0.030 mole n-butylithium in 200 mL THF and stirred for two hours at room temperature. Then 0.030 mole 6-(dimethyl)aminofulvene was added and the mixture was stirred for five hours. The deep red solution was then reacted with 0.060 mole methyllithium and the mixture was refluxed for 8 to 10 hours to form a dianion. The reaction product was hydrolysed very slowly with cooling. The reaction vessel was cooled in a dry ice bath and the reaction mixture was hydrolysed by very slow dropping of a solution of aqueous HCl in THF. The thus produced CHMe-bridged ligand was extracted with pentane, dried over sodium sulfate, and the solvent was evaporated.

1. stirringthe mixture was stirred for five hours
2. temperaturethe mixture was refluxed for 8 to 10 hours
3. customto form a dianion
4. temperaturewith cooling
5. temperatureThe reaction vessel was cooled in a dry ice bath
6. extractionThe thus produced CHMe-bridged ligand was extracted with pentane
7. dry with materialdried over sodium sulfate
8. customthe solvent was evaporated