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

HRID 1493072

反応式

HRID 1493072 の反応式
[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>O1CCCC1.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

参加物

7

反応物 4

HCID 6853FluoreneHCID 8058HexaneHCID 22238549Diphenyl FulveneHCID 178418339Butyllithium

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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 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 residue was left to crystallize at -35° C. 5.1 g (42%) of 1,1-cyclopentadienyl(9-fluorenyl)diphenylmethane were obtained as a beige powder.

後処理

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

出典と根拠

ORDレコード
ord-d58657b61e5444edab7720b812f48d43
出典データセット
uspto-grants-1994_12
特許番号
US05376725

関連ノート

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