Hydrogen Peroxide → 2-Bromo-6-methylpyridine 1-oxide

HRID 1775371

반응식

HRID 1775371 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N:3]=1.[OH:9]O>C(O)(=O)C.O>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N+:3]=1[O-:9]

참가 물질

5

반응물 2

HCID 784Hydrogen PeroxideHCID 792052-Bromo-6-methylpyridine

생성물 1

HCID 36520842-Bromo-6-methylpyridine 1-oxide수율 95%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

2-Bromo-6-methylpyridine (36 g, 0.2 mol) was dissolved in acetic acid (700 ml), hydrogen peroxide (30%, 62 ml, 0.6 mol) was added and the mixture was stirred at 90° C. for 24 hours. After cooling to room temperature, the mixture was diluted with water (700 ml) and extracted with DCM (4×). The combined organic phases were washed with water, dried (sodium sulfate) and concentrated under reduced pressure to give 36 g of a red-brown liquid (0.19 mol, 94%) MS (APCI) m/z=188.0 [M+1]+.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with DCM (4×)
  3. washThe combined organic phases were washed with water
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-33318d8f82124ebab379a60e6bb149be
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09260441B2

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