반응 #1463847

ord-2ba957d05f104a3588cc47ed587a0aa0

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타as a result of which the solution
  2. 2
    추출the solution was extracted with ether
  3. 3
    건조The ether phase was dried over MgSO4
  4. 4
    농축concentrated
  5. 5
    기타to 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05663268uspto-grants-1997_09