Hydrogen peroxide water → Pyridine, 4-chloro-3-methoxy-2-methyl-, 1-oxide

HRID 1061439

반응식

HRID 1061439 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([CH3:8])[C:3]=1[O:9][CH3:10].[OH2:11].OO>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][N+:5]([O-:11])=[C:4]([CH3:8])[C:3]=1[O:9][CH3:10]

참가 물질

4

반응물 2

HCID 449047Hydrogen peroxide waterHCID 105830464-Chloro-3-methoxy-2-methylpyridine

생성물 1

HCID 5083929Pyridine, 4-chloro-3-methoxy-2-methyl-, 1-oxide

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
90 °C

실험 절차

36.98 g of 4-chloro-3-methoxy-2-methylpyridine (V) was dissolved in 685 ml of acetic acid and 92 ml of hydrogen peroxide water was added thereto and the resulting mixture was heated at 90° C. for 24 hours, and thereafter, the reaction solution was distilled off under reduced pressure. The resulting residue was dissolved in chloroform and washed with saturated sodium bicarbonate solution, and saturated salt water, and thereafter, dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 37.64 g of 4-chloro-3-methoxy-2-methylpyridine N-oxide (VI).

후처리

  1. distillationthe reaction solution was distilled off under reduced pressure
  2. dissolutionThe resulting residue was dissolved in chloroform
  3. washwashed with saturated sodium bicarbonate solution, and saturated salt water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-33f6df645d154677aa5c5b80a33a661c
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525066B2

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