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

HRID 50552
ノート
印刷プレビュー

反応式

HRID 50552 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
参加物実験手順後処理出典と根拠反応ノート

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 8028
Tetrahydrofuran
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-7088ca75658747c6aa2a2c7432e03144
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06713426B1

反応ノート

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