Phosphorus oxychloride → 4-Chloro-3-methoxy-2-methylpyridine

HRID 649209

반응식

HRID 649209 반응식
[CH3:1][O:2][C:3]1[C:8](=O)[CH:7]=[CH:6][NH:5][C:4]=1[CH3:10].P(Cl)(Cl)([Cl:13])=O>>[Cl:13][C:8]1[CH:7]=[CH:6][N:5]=[C:4]([CH3:10])[C:3]=1[O:2][CH3:1]

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 3234243-Methoxy-2-methyl-1H-pyridin-4-one

생성물 1

HCID 105830464-Chloro-3-methoxy-2-methylpyridine

실험 절차

3-Methoxy-2-methyl-4(1H)-pyridone (5.6 g) was suspended in phosphorus oxychloride (50 ml), refluxed for 10 hours, and concentrated. To the resultant residue was added toluene and the residual phosphorus oxychloride was evaporated under reduced pressure. To the resultant oily substance were added chloroform and water and the chloroform layer was separated. The aqueous layer was made alkaline with potassium carbonate and extracted with chloroform. The chloroform solutions thus obtained were combined, washed with water, dried, and evaporated. The residue was purified by column chromatography on silica gel, to give 4-chloro-3-methoxy-2-methylpyridine (4.8 g) as a light brown oil.

후처리

  1. temperaturerefluxed for 10 hours
  2. concentrationconcentrated
  3. additionTo the resultant residue was added toluene
  4. customthe residual phosphorus oxychloride was evaporated under reduced pressure
  5. additionTo the resultant oily substance were added chloroform and water
  6. customthe chloroform layer was separated
  7. extractionextracted with chloroform
  8. customThe chloroform solutions thus obtained
  9. washwashed with water
  10. customdried
  11. customevaporated
  12. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-f14632ad3c684d5caf7fc9c6037bd456
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04738975

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