9-(2-bromoethyl)-9H-fluorene → HCID 86752827、化合物

HRID 1955286

反応式

HRID 1955286 の反応式
[CH:1]([C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][C:5]=2[CH:4]=1)=[CH2:2].C([Li])CCC.Br[CH2:22][CH2:23][CH:24]1[C:36]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[C:30]2[C:25]1=[CH:26][CH:27]=[CH:28][CH:29]=2>C(OCC)C>[CH:1]([C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][C:5]=2[C:4]=1[C:24]1([CH2:23][CH3:22])[C:36]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[C:30]2[C:25]1=[CH:26][CH:27]=[CH:28][CH:29]=2)=[CH2:2]

参加物

5

反応物 3

HCID 110002159-(2-bromoethyl)-9H-fluoreneHCID 110416072-ethenyl-9H-fluoreneHCID 178418339Butyllithium

生成物 1

HCID 86752827HCID 86752827、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To 1.15 g (6.0 mmol) 2-vinylfluorene in 100 mL diethyl ether was added 3.75 mL (6.0 mmol) n-butyllithium (1.6M in hexane). The reaction mixture was stirred for 4 hours at room temperature. Then 1.64 g (6.0 mmol) 1-bromo-2-(9-fluorenyl)ethane was added and the mixture was stirred for 14 hours at room temperature. The precipitate was removed by filtration, washed with methanol, filtered with pentane using silica gel 60, and concentrated by evaporation under vacuum. The yield was 1.69 g (73%) 1-(9-(2-vinyl)fluorenyl)-2-(9-fluorenyl)ethane as a colorless solid.

後処理

  1. stirringthe mixture was stirred for 14 hours at room temperature
  2. customThe precipitate was removed by filtration
  3. washwashed with methanol
  4. filtrationfiltered with pentane
  5. concentrationconcentrated by evaporation under vacuum

出典と根拠

ORDレコード
ord-188e5440bfd343b7bbf8113769096646
出典データセット
uspto-grants-2000_09
特許番号
US06124414

関連ノート

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