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

HRID 845541노트

반응식

HRID 845541 반응식
[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

참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 30152703-Methoxy-2-methylpyridine

생성물 1

HCID 122140163-Methoxy-2-methylpyridine 1-oxide수율 60%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3c8d6b5193b74c0c803784307d37c20c
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04758579

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