반응 #1463847
ord-2ba957d05f104a3588cc47ed587a0aa0
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후처리
- 1기타as a result of which the solution
- 2추출the solution was extracted with ether
- 3건조The ether phase was dried over MgSO4
- 4농축concentrated
- 5기타to crystallize at -35° C
실험 절차
Diphenylenemethylene(9-fluorenyl)(cyclopentadienyl)zirconium dichloride ##STR11## 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 THF 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, as a result of which the solution turns yellow, and the solution was extracted with ether. The ether phase was dried over MgSO4, concentrated, and allowed to crystallize at -35° C. 5.1 g (42%) of 1,1-cyclopentadienyl-(9-fluorenyl)diphenylmethane was obtained as a beige powder.