Water → 1,1-Cyclopentadienyl(9-fluorenyl)dipenylmethane

HRID 2253854

반응식

HRID 2253854 반응식
[CH2:1]([Li])[CH2:2][CH2:3][CH3:4].[CH:6]1[C:18]2[CH2:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]=2[CH:9]=[CH:8][CH:7]=1.[C:19]1([C:25]2[CH:29]=[CH:28][C:27](=[CH2:30])[C:26]=2[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)C=CC=CC=1.O.[CH3:38]CCCCC>O1CCCC1.[Cl-].[Cl-].C1(C(=[Zr+2](C2C3C=CC=CC=3C3C2=CC=CC=3)C2C=CC=C2)C2C=CC=CC=2)C=CC=CC=1>[C:4]1([C:26]([CH:17]2[C:16]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[C:10]3[C:18]2=[CH:6][CH:7]=[CH:8][CH:9]=3)([C:25]2[CH:19]=[CH:30][CH:27]=[CH:28][CH:29]=2)[C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)[CH2:38][CH2:1][CH2:2][CH:3]=1

참가 물질

8

반응물 5

HCID 962WaterHCID 6853FluoreneHCID 8058HexaneHCID 22238549Diphenyl FulveneHCID 178418339Butyllithium

생성물 1

HCID 227351321,1-Cyclopentadienyl(9-fluorenyl)dipenylmethane수율 42%

시약·촉매·용매 2

HCID 178420589HCID 178420589, 화합물촉매HCID 8028Tetrahydrofuran용매

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.

후처리

  1. extractionthe solution was extracted with ether
  2. dry with materialThe ether phase was dried over MgSO4
  3. concentrationconcentrated
  4. waitthe concentrate was left
  5. customto crystallize at -35° C

출처 및 근거

ORD 기록
ord-162d04fd3c194e18bd2a055ac47bf836
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05232993

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