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

HRID 973479ノート

反応式

HRID 973479 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 pH7, 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-2bb7d90837654a9eb1be25c5fd3ffa53
出典データセット
uspto-grants-1991_11
特許番号
US05063237

反応ノート

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