Hydrogen Peroxide → 5-Methoxy-2-methyl-1-oxo-1lambda~5~-pyridine

HRID 845533노트

반응식

HRID 845533 반응식
[OH:1]O.[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([CH3:11])=[N:9][CH:10]=1>C(O)(=O)C>[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([CH3:11])=[N+:9]([O-:1])[CH:10]=1

참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 133587775-Methoxy-2-methylpyridine

생성물 1

HCID 122140195-Methoxy-2-methyl-1-oxo-1lambda~5~-pyridine수율 77%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

120 g of 30% strength hydrogen peroxide solution are added dropwise to a solution of 60.9 g of 5-methoxy-2-methylpyridine in 300 ml of glacial acetic acid at 60° C. in the course of 1 hour and the mixture is subsequently stirred for 3 hours. After destruction of excess per-compounds by addition of active manganese dioxide, the mixture is filtered, the filtrate is concentrated, the residue is clarified hot in 500 ml of ethyl acetate, the mixture is concentrated again and the residue is distilled under 0.3 mbar. 54 g (77% of theory) of 5-methoxy-2-methylpyridine 1-oxide are obtained as a rapidly solidifying oil (b.p. 130° C.); m.p. 80°-84° C.

후처리

  1. customAfter destruction of excess per-compounds
  2. additionby addition of active manganese dioxide
  3. filtrationthe mixture is filtered
  4. concentrationthe filtrate is concentrated
  5. concentrationthe mixture is concentrated again
  6. distillationthe residue is distilled under 0.3 mbar

출처 및 근거

ORD 기록
ord-cb46f12517d842b19906d830bd4b49e3
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04758579

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