Phosphorus oxychloride → 2-Chloro-4-methyl-3-nitropyridine

HRID 53518노트

반응식

HRID 53518 반응식
O[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:13].P(Cl)(Cl)(Cl)=O>>[Cl:13][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[CH:5]=[CH:4][N:3]=1

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 178428606HCID 178428606, 화합물

생성물 1

HCID 3453632-Chloro-4-methyl-3-nitropyridine

실험 절차

A mixture of 25 g of 2-hydroxy-4-methyl-3-nitropyridine, 12.5 g of phosphorous pentachloride, and 62 ml of phosphorous oxychloride was refluxed for 2 hrs. After cooling, the mixture was poured onto crushed ice and stirred until a precipitate formed. The product was extracted with methylene chloride, dried (sodium sulfate) and concentrated to a brown oil, which was washed with hot hexane. Concentration in vacuo provided 16.2 g of the the title compound, m.p. 45°-47° C.

후처리

  1. temperaturewas refluxed for 2 hrs
  2. temperatureAfter cooling
  3. additionthe mixture was poured
  4. customonto crushed ice
  5. customformed
  6. extractionThe product was extracted with methylene chloride
  7. dry with materialdried (sodium sulfate)
  8. concentrationconcentrated to a brown oil, which
  9. washwas washed with hot hexane
  10. concentrationConcentration in vacuo

출처 및 근거

ORD 기록
ord-73144cc5669447789f248444d3d67268
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620974

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