Sodium Dichromate → 2,7-Bis(1-oxo-4-(1-piperidyl)butyl)-9H-fluoren-9-one

HRID 441640ノート

反応式

HRID 441640 の反応式
[N:1]1([CH2:7][CH2:8][CH2:9][C:10]([C:12]2[CH:24]=[CH:23][C:22]3[C:21]4[C:16](=[CH:17][C:18]([C:25](=[O:35])[CH2:26][CH2:27][CH2:28][N:29]5[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]5)=[CH:19][CH:20]=4)[CH2:15][C:14]=3[CH:13]=2)=[O:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=[O:37].[Na+].[Na+]>C(O)(=O)C>[N:1]1([CH2:7][CH2:8][CH2:9][C:10]([C:12]2[CH:24]=[CH:23][C:22]3[C:21]4[C:16](=[CH:17][C:18]([C:25](=[O:35])[CH2:26][CH2:27][CH2:28][N:29]5[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34]5)=[CH:19][CH:20]=4)[C:15](=[O:37])[C:14]=3[CH:13]=2)=[O:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 25408Sodium DichromateHCID 1602411,1'-(9H-Fluorene-2,7-diyl)bis(4-(1-piperidinyl)-1-butanone)

生成物 1

HCID 1475842,7-Bis(1-oxo-4-(1-piperidyl)butyl)-9H-fluoren-9-one

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 9.0 g (0.019 mole) 2,7-bis(4-piperidinobutyryl)fluorene, 7.54 g (0.0253 mole) sodium dichromate and 300 ml of glacial acetic acid is stirred and refluxed for one hour. The reaction mixture is evaporated to semi-dryness and made basic using concentrated ammonium hydroxide. The solid which precipitates is filtered, washed with water and chromatographed on alumina using chloroform as the eluant. The solvent is removed from the fraction collected, leaving a solid residue which is recrystallized three times from chloroform-acetone to yield 2,7-bis(4-piperidinobutyryl)fluoren-9-one, M.P. 168°-170° C.

後処理

  1. temperaturerefluxed for one hour
  2. customThe reaction mixture is evaporated to semi-dryness
  3. customThe solid which precipitates
  4. filtrationis filtered
  5. washwashed with water
  6. customchromatographed on alumina
  7. customThe solvent is removed from the fraction
  8. customcollected
  9. customleaving a solid residue which
  10. customis recrystallized three times from chloroform-acetone

出典と根拠

ORDレコード
ord-2c5e5fac72234c60a8b404ac55c92c56
出典データセット
uspto-grants-1977_08
特許番号
US04041165

反応ノート

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