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

HRID 845533ノート

反応式

HRID 845533 の反応式
[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

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 133587775-Methoxy-2-methylpyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cb46f12517d842b19906d830bd4b49e3
出典データセット
uspto-grants-1988_07
特許番号
US04758579

反応ノート

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