Acetic Acid → 9H-fluorene-2-carbonitrile

HRID 1678372ノート

反応式

HRID 1678372 の反応式
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][C:2]=1[CH:14]=O.C([O-])(=O)C.[Na+].[Cl-].O[NH3+:23].C(O)(=O)C>O>[C:14]([C:2]1[CH:3]=[CH:4][C:5]2[C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[CH2:12][C:13]=2[CH:1]=1)#[N:23]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 21645Hydroxylamine HClHCID 34804Fluorene-2-carboxaldehydeHCID 517045Sodium Acetate

生成物 1

HCID 173029H-fluorene-2-carbonitrile収率 63.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

25 g of 2-fluorenecarboaldehyde, 11.6 g of sodium acetate, 9.7 g of hydroxy ammonium chloride and 150 ml of acetic acid were stirred at 130 for 18 hours. The reaction mixture was allowed to room temperature, poured into 200 ml of water and the precipitate was collected by filtration. The crude product was purified by column chromatography, giving 15.57 g (63%) of 2-cyanofluorene.

後処理

  1. customwas allowed to room temperature
  2. filtrationthe precipitate was collected by filtration
  3. customThe crude product was purified by column chromatography

出典と根拠

ORDレコード
ord-c38194389ac749a1a244c711695c52a3
出典データセット
uspto-grants-2011_08
特許番号
US08008507B2

反応ノート

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