Water → N-Acetyl-N-(3-aminophenethyl)amine

HRID 1173126ノート

反応式

HRID 1173126 の反応式
[C:1]([NH:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-])=O)[CH:8]=1)(=[O:3])[CH3:2].C([O-])(=O)C.[NH4+].O>C(O)C.[Fe]>[C:1]([NH:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH2:13])[CH:8]=1)(=[O:3])[CH3:2]

参加物

6

反応物 3

HCID 962WaterHCID 517165Ammonium AcetateHCID 22674066N-(3-Nitrophenethyl)acetamide

生成物 1

HCID 22674097N-Acetyl-N-(3-aminophenethyl)amine収率 96%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

実験手順

N-Acetyl-N-(3-nitrophenethyl)amine (2.1 g, Production Example 28b) was dissolved in ethanol (40 ml). To the mixture were added an iron powder (2.25 g), ammonium acetate (4.3 g) and water (20 ml), followed by heating under reflux for 1.5 hours. Solid was filtered off and washed with ethanol, and then the filtrate was partially evaporated. The residue was extracted with ethyl acetate, washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, to give the title compound (1.723 g, 96%) as a yellow oil.

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 1.5 hours
  3. filtrationSolid was filtered off
  4. washwashed with ethanol
  5. customthe filtrate was partially evaporated
  6. extractionThe residue was extracted with ethyl acetate
  7. washwashed with brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-af677a9849a940ed8aff78446c6cbdf0
出典データセット
uspto-grants-2010_11
特許番号
US07834049B2

反応ノート

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