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

HRID 1081976

반응식

HRID 1081976 반응식
[CH3:1]CCCCC.[CH2:7]([Li])[CH2:8][CH2:9][CH3:10].[CH:12]1[C:24]2[CH2:23][C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16]=2[CH:15]=[CH:14][CH:13]=1.[C:25]1([C:31]2[CH:35]=[CH:34][C:33](=[CH2:36])[C:32]=2[C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)C=CC=CC=1>C1COCC1.O>[C:10]1([C:32]([CH:23]2[C:22]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:16]3[C:24]2=[CH:12][CH:13]=[CH:14][CH:15]=3)([C:31]2[CH:25]=[CH:36][CH:33]=[CH:34][CH:35]=2)[C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)[CH2:1][CH2:7][CH2:8][CH:9]=1

참가 물질

7

반응물 4

HCID 6853FluoreneHCID 8058HexaneHCID 22238549Diphenyl FulveneHCID 178418339Butyllithium

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

12.3 cm3 (30.7 mmol) of a 2.5 molar hexane solution of n-butyllithium were added slowly at room temperature to a solution of 5.10 g (30.7 mmol) of fluorene in 60 cm3 of THF. 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, the solution becoming a yellow color, and the solution was extracted with ether. The ether phase was dried over MgSO4, evaporated and left to crystallize at -35° C. 5.1 g (42%) of 1,1-cyclopentadienyl(9-fluorenyl)dipenylmethane 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. customevaporated
  4. waitleft
  5. customto crystallize at -35° C

출처 및 근거

ORD 기록
ord-0575f94ca7944391ae03911a9e71a1e2
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05587501

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