Sodium → 2-Methoxy-5-nitropyridine-3-carboxylic acid

HRID 1038453ノート

反応式

HRID 1038453 の反応式
Cl[C:2]1[N:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH3:14][O-:15].[Na+].[Na]>CO>[CH3:14][O:15][C:2]1[N:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

5

反応物 3

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 125426642-Chloro-5-nitronicotinic acid

生成物 1

HCID 207150902-Methoxy-5-nitropyridine-3-carboxylic acid収率 73%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

To 2-chloro-5-nitro-nicotinic acid (1.0 mmol) in methanol was added a solution of sodium methoxide in methanol (2.4 mmol, freshly prepared from sodium metal in methanol). The solution was refluxed for 2 h and the mixture was allowed to cool and concentrated in vacuo. To the resulting residue was added 10% citric acid solution (20 ml) and the solution extracted with ethyl acetate (20 ml). The organic layer was dried (MgSO4) and concentrated in vacuo. The residue was crystallised from water to give a yellow-white solid (73%).

後処理

  1. temperatureThe solution was refluxed for 2 h
  2. temperatureto cool
  3. concentrationconcentrated in vacuo
  4. additionTo the resulting residue was added 10% citric acid solution (20 ml)
  5. extractionthe solution extracted with ethyl acetate (20 ml)
  6. dry with materialThe organic layer was dried (MgSO4)
  7. concentrationconcentrated in vacuo
  8. customThe residue was crystallised from water

出典と根拠

ORDレコード
ord-488cacb08ca14f5ca7eaf8e7806302ec
出典データセット
uspto-grants-2013_10
特許番号
US08551990B2

反応ノート

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