반응 #2341036

반응 방정식

diphenylfulvene

n-butyllithium

fluorene

hexane

water

→

1,1-cyclopentadienyl-(9-fluorenyl)diphenylmethane

수율 42.0%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   추출the solution was extracted with ether
2. 2
   건조The ether phase was dried over MgSO4
3. 3
   농축concentrated
4. 4
   workup.WAITthe concentrate was left
5. 5
   기타to crystallize at -35° C

실험 절차

Diphenylmethylene(9-fluorenyl)(cyclopentadienyl)zirconium dichloride ##STR11## 12.3 cm3 (30.7 mmol) of a 2.5 molar solution of n-butyllithium in hexane 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 in color, and the solution was extracted with ether. The ether phase was dried over MgSO4 and concentrated and the concentrate was left to crystallize at -35° C. 5.1 g (42%) of 1,1-cyclopentadienyl-(9-fluorenyl)diphenylmethane were obtained as a beige powder.

출처