Ethylamine → N-Ethyl-3-nitropyridin-4-amine

HRID 1817147ノート

反応式

HRID 1817147 の反応式
Cl.CO[C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[N+:10]([O-:12])=[O:11].[CH2:13]([NH2:15])[CH3:14]>C(O)C.O>[CH2:13]([NH:15][C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[N+:10]([O-:12])=[O:11])[CH3:14]

参加物

5

反応物 2

HCID 6341EthylamineHCID 3558314-Methoxy-3-nitropyridine hydrochloride

生成物 1

HCID 21937597N-Ethyl-3-nitropyridin-4-amine収率 96%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

4-Methoxy-3-nitropyridine hydrochloride (11.2 g, 58.9 mmol) in ethanol (75 ml) was treated with a 70% solution of ethylamine in water (64 ml) and heated under reflux for 2 hours. After cooling to room temperature, the solvent was removed in vacuo and the residue dissolved in ethyl acetate and water. The mixture was extracted (×3) with ethyl acetate, washed with water and saturated aqueous sodium chloride solution before drying over magnesium sulfate. Evaporation of the solvent afforded the title compound (11.7 g, 96%).

後処理

  1. temperatureheated
  2. temperatureunder reflux for 2 hours
  3. customthe solvent was removed in vacuo
  4. dissolutionthe residue dissolved in ethyl acetate
  5. extractionThe mixture was extracted (×3) with ethyl acetate
  6. washwashed with water and saturated aqueous sodium chloride solution
  7. dry with materialbefore drying over magnesium sulfate
  8. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-c98222fc8f0f467294076e546512ad1b
出典データセット
uspto-grants-2009_10
特許番号
US07598251B2

反応ノート

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