Phosphorus oxychloride → 4-Chloro-2,6-dimethyl-3-nitropyridine

HRID 892769ノート

反応式

HRID 892769 の反応式
[CH3:1][C:2]1[CH:7]([N+:8]([O-:10])=[O:9])[C:6](=O)[CH:5]=[C:4]([CH3:12])[N:3]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:6]1[CH:5]=[C:4]([CH3:12])[N:3]=[C:2]([CH3:1])[C:7]=1[N+:8]([O-:10])=[O:9]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 781987842,6-Dimethyl-3-nitro-4-pyridone

生成物 1

HCID 107027254-Chloro-2,6-dimethyl-3-nitropyridine

実験手順

By the method of Yakugaku Zasshi, 87, 387 (1967), 2,6-dimethyl-3-nitro-4-pyridone (11.23 g, 66.8 mmol) and phosphorus oxychloride (57 ml) were heated together at reflux for 11/2 hours. The excess reagent was removed under reduced pressure, and the residue dissolved in dichloromethane (150 ml). This solution was treated with dilute aqueous sodium bicarbonate until the aqueous layer was at pH 7, and then the organic phase was separated, dried (MgSO4) and concentrated under reduced pressure to give a pale yellow solid, (9.8 g, 79%). Caution: this compound is believed to be a powerful skin irritant.

後処理

  1. temperatureat reflux for 11/2 hours
  2. customThe excess reagent was removed under reduced pressure
  3. dissolutionthe residue dissolved in dichloromethane (150 ml)
  4. additionThis solution was treated with dilute aqueous sodium bicarbonate until the aqueous layer
  5. customthe organic phase was separated
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated under reduced pressure
  8. customto give a pale yellow solid, (9.8 g, 79%)

出典と根拠

ORDレコード
ord-fa9575c72e164083b4cc7253f965c478
出典データセット
uspto-grants-1992_06
特許番号
US05120747

反応ノート

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