Phosphorus pentachloride → 2-Chloro-5-ethyl-6-methyl-3-nitropyridine

HRID 1033004ノート

反応式

HRID 1033004 の反応式
[N+:1]([C:4]1[C:5](=O)[NH:6][C:7]([CH3:12])=[C:8]([CH2:10][CH3:11])[CH:9]=1)([O-:3])=[O:2].P(Cl)(Cl)(Cl)(Cl)[Cl:15]>C(Cl)(Cl)Cl>[Cl:15][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][C:8]([CH2:10][CH3:11])=[C:7]([CH3:12])[N:6]=1

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 103523142(1H)-Pyridinone, 5-ethyl-6-methyl-3-nitro-

生成物 1

HCID 103755472-Chloro-5-ethyl-6-methyl-3-nitropyridine収率 67%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
140 °C

実験手順

A mixture of 3-nitro-5-ethyl-6-methylpyridin-2(1H)-one (0.91 g, 5.0 mmol) and phosphorus pentachloride (1.25 g, 6.0 mmol), under a nitrogen atmosphere, was heated at 140° C. for 0.5 hours. The cooled mixture was diluted with chloroform and ice water. The separated chloroform layer was then washed with water, saturated aqueous NaHCO3 and dried (Na2SO4). After filtering through a pad of charcoal, solvent was evaporated to yield 672 mg (67%) of product.

後処理

  1. washThe separated chloroform layer was then washed with water, saturated aqueous NaHCO3
  2. dry with materialdried (Na2SO4)
  3. filtrationAfter filtering through a pad of charcoal, solvent
  4. customwas evaporated

出典と根拠

ORDレコード
ord-3861344d06fa41ed90f224e026380e4b
出典データセット
uspto-grants-1994_05
特許番号
US05308854

反応ノート

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