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

HRID 53518ノート

反応式

HRID 53518 の反応式
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

参加物

4

反応物 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 178428606HCID 178428606、化合物

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-73144cc5669447789f248444d3d67268
出典データセット
uspto-grants-1997_04
特許番号
US05620974

反応ノート

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