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

HRID 1914598노트

반응식

HRID 1914598 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 207150902-Methoxy-5-nitropyridine-3-carboxylic acid수율 73%

시약·촉매·용매 1

HCID 887Methanol용매3회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-b4e30ef08e6847a1b8a7d5dd57fbea0a
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614212B2

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