2,3-Lutidine → Pyridine, 2,3-dimethyl-, 1-oxide

HRID 35446

反応式

HRID 35446 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N:3]=1.ClC1C=CC=C(C(OO)=[O:17])C=1>C(Cl)Cl>[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:17]

参加物

4

反応物 2

HCID 114202,3-LutidineHCID 70297m-Chloroperbenzoic acid

生成物 1

HCID 3840573Pyridine, 2,3-dimethyl-, 1-oxide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 24 g (0.22 mol) of 2,3-dimethylpyridine in 100 ml of methylene chloride is treated while cooling with ice with a solution of 46.6 g (0.27 mol) of m-chloroperbenzoic acid in 100 ml of methylene chloride. The reaction mixture is heated under reflux for 2 hours and concentrated in a rotary evaporator. The residue is chromatographed on silica gel with ethyl acetate/methylene chloride (3:1) as the elution agent, the medium pressure flash chromatography method being used and the pressure being produced with nitrogen gas. By recrystallization from ether there is obtained 2,3-dimethylpyridine 1-oxide of melting point 56°.

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux for 2 hours
  3. concentrationconcentrated in a rotary evaporator
  4. customThe residue is chromatographed on silica gel with ethyl acetate/methylene chloride (3:1) as the elution agent
  5. customthe pressure being produced with nitrogen gas
  6. customBy recrystallization from ether

出典と根拠

ORDレコード
ord-39749d82d8984a9b830f19e45fb8b4be
出典データセット
uspto-grants-1988_08
特許番号
US04766133

関連ノート

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