Hydrogen Peroxide → 5-Methoxycarbonylpyridine-2-carboxylic acid 1-oxide

HRID 976026노트

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HRID 976026 반응식
[N:1]1[CH:6]=[C:5]([C:7]([O:9][CH3:10])=[O:8])[CH:4]=[CH:3][C:2]=1[C:11]([O:13]C)=[O:12].[OH:15]O>C(O)(=O)C>[CH3:10][O:9][C:7]([C:5]1[CH:6]=[N+:1]([O-:15])[C:2]([C:11]([OH:13])=[O:12])=[CH:3][CH:4]=1)=[O:8]

참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 234911Dimethyl 2,5-pyridine dicarboxylate

생성물 1

HCID 199603735-Methoxycarbonylpyridine-2-carboxylic acid 1-oxide

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
20 °C

실험 절차

12 g (60 mmol) of dimethyl pyridine-2,5-dicarboxylate were suspended in 30 ml of glacial acetic acid and treated with 13 ml of hydrogen peroxide (35%) at 20° C. with stirring. The mixture was then heated with stirring to 100° C. (internal temperature), a clear solution being formed at 50° C. After the mixture had been stirred at 100° C. for 90 min, it was allowed to cool to 20° C., the crystalline precipitate was filtered off with suction and washed with water and, after drying, 7.5 g of product were obtained, m.p. 160° C. (dec.).

후처리

  1. temperatureThe mixture was then heated
  2. stirringwith stirring to 100° C. (internal temperature)
  3. customa clear solution being formed at 50° C
  4. stirringAfter the mixture had been stirred at 100° C. for 90 min
  5. filtrationthe crystalline precipitate was filtered off with suction
  6. washwashed with water
  7. customafter drying

출처 및 근거

ORD 기록
ord-5cbb5018f78a4c2ca43a5871c1338083
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05610172

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