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p-Nitroacetophenone → p-Aminoacetophenone

HRID 45664
ノート
印刷プレビュー

反応式

HRID 45664 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:12])[CH3:11])=[CH:6][CH:5]=1)([O-])=O.[NH4+].[Cl-]>C(O)C.O.[Fe]>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:12])[CH3:11])=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 7487p-NitroacetophenoneHCID 25517Ammonium Chloride

生成物 1

HCID 7468p-Aminoacetophenone収率 63.1%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Into a 100-mL 3-necked round-bottom flask, was placed a solution of 1-(4-nitrophenyl)ethanone (6 g, 36.36 mmol, 1.00 equiv) in ethanol (100 mL), water (15 mL). This was followed by the addition of NH4Cl (3.85 g, 72.64 mmol, 2.00 equiv) in several batches. To this was added Fe (10.18 g, 181.79 mmol, 5.00 equiv) in several batches, while the temperature was maintained at reflux. The resulting mixture was heated to reflux for 2 h. The solids were filtered out and the resulting filtrate was concentrated under vacuum. The residue was diluted with 50 mL of water. The resulting solution was extracted with 3×50 mL of ethyl acetate and the organic layers combined and dried over anhydrous sodium sulfate and concentrated under vacuum to give 3.1 g (60%) of 1-(4-aminophenyl)ethanone as a yellow solid.

後処理

  1. customInto a 100-mL 3-necked round-bottom flask, was placed
  2. temperaturewhile the temperature was maintained
  3. temperatureat reflux
  4. temperatureThe resulting mixture was heated
  5. temperatureto reflux for 2 h
  6. filtrationThe solids were filtered out
  7. concentrationthe resulting filtrate was concentrated under vacuum
  8. additionThe residue was diluted with 50 mL of water
  9. extractionThe resulting solution was extracted with 3×50 mL of ethyl acetate
  10. dry with materialdried over anhydrous sodium sulfate
  11. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-07dedcf575804d12ae737fff1c6788ab
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08541448B2

反応ノート

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