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

HRID 1005683ノート

反応式

HRID 1005683 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

In ethanol (40 ml) was dissolved 2.1 g of N-acetyl-N-(3-nitrophenethyl)amine (Preparation Example 28), and powdered iron (2.25 g), ammonium acetate (4.3 g) and water (20 ml) were added thereto, followed by heating under reflux for 1.5 hours. The solid matter was filtered off and washed with ethanol, and a part of the filtrate was evaporated. The residue was extracted with ethyl acetate, washed with brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give the title compound (1.723 g, 96%) as a yellow oil.

後処理

  1. additionwere added
  2. temperatureby heating
  3. temperatureunder reflux for 1.5 hours
  4. filtrationThe solid matter was filtered off
  5. washwashed with ethanol
  6. customa part of the filtrate was evaporated
  7. extractionThe residue was extracted with ethyl acetate
  8. washwashed with brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-49e02630b8ae4d999313e885843b385c
出典データセット
uspto-grants-2004_09
特許番号
US06787534B2

反応ノート

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