Hydrogen Peroxide → 3-Methoxy-2-methylpyridine 1-oxide

HRID 845541

反応式

HRID 845541 の反応式
[CH3:1][O:2][C:3]1[C:4]([CH3:9])=[N:5][CH:6]=[CH:7][CH:8]=1.[OH:10]O>C(O)(=O)C>[CH3:1][O:2][C:3]1[C:4]([CH3:9])=[N+:5]([O-:10])[CH:6]=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 30152703-Methoxy-2-methylpyridine

生成物 1

HCID 122140163-Methoxy-2-methylpyridine 1-oxide収率 60%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

15.3 g (0.124 mole) of 3-methoxy-2-methylpyridine are dissolved in 100 ml of glacial acetic acid, and 40 ml of 30% strength hydrogen peroxide are added in 4 portions at 80° C. in the course of 6 hours. The mixture is stirred for a further three hours and then concentrated in vacuo (1.5 kPa), and two 50 ml portions of acetic acid are added, the mixture being concentrated completely after each addition. Following negative detection of per-compounds, the mixture is distilled in a bulb tube oven. The fraction which distills at 120° C. (1.5 Pa) is extracted by stirring in a little diethyl ether and the solid is filtered off and dried. 12 g (60% of theory) of 3-methoxy-2-methylpyridine 1-oxide are obtained in the form of colorless crystals of m.p. 72°-78° C.

後処理

  1. concentrationconcentrated in vacuo (1.5 kPa), and two 50 ml portions of acetic acid
  2. additionare added
  3. concentrationthe mixture being concentrated completely
  4. additionafter each addition
  5. distillationthe mixture is distilled in a bulb tube oven
  6. distillationThe fraction which distills at 120° C. (1.5 Pa)
  7. extractionis extracted
  8. stirringby stirring in a little diethyl ether
  9. filtrationthe solid is filtered off
  10. customdried

出典と根拠

ORDレコード
ord-3c8d6b5193b74c0c803784307d37c20c
出典データセット
uspto-grants-1988_07
特許番号
US04758579

関連ノート

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