Hydrogen Peroxide → Ethyl 6-methyl-1-oxo-1lambda~5~-pyridine-3-carboxylate

HRID 1030510

반응식

HRID 1030510 반응식
[CH3:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][N:3]=1.[OH:13]O>C(O)(=O)C>[CH2:9]([O:8][C:6]([C:5]1[CH:11]=[CH:12][C:2]([CH3:1])=[N+:3]([O-:13])[CH:4]=1)=[O:7])[CH3:10]

참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 281994Ethyl 6-methylnicotinate

생성물 1

HCID 15045502Ethyl 6-methyl-1-oxo-1lambda~5~-pyridine-3-carboxylate

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

A mixture of 14.9 g of ethyl 6-methylnicotinate, 60 ml of acetic acid and 21.5 ml of 30% hydrogen peroxide was stirred at 80° C. for 16 hours, the reaction liquid was concentrated under a reduced pressure, water was added to the concentrate, and the mixture was extracted with chloroform. The chloroform layer was washed with an aqueous solution of potassium carbonate and dried over anhydrous potassium carbonate, and the solvent was removed under a reduced pressure to obtain 14.0 g of 5-ethoxycarbonyl-2-methyl pyridine-1-oxide. ##STR6##

후처리

  1. customthe reaction liquid
  2. concentrationwas concentrated under a reduced pressure, water
  3. additionwas added to the concentrate
  4. extractionthe mixture was extracted with chloroform
  5. washThe chloroform layer was washed with an aqueous solution of potassium carbonate
  6. dry with materialdried over anhydrous potassium carbonate
  7. customthe solvent was removed under a reduced pressure

출처 및 근거

ORD 기록
ord-ee29a6252c3b4ec497a0dca1f09e593b
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05106859

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