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

HRID 1033004Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1033004
[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

Komponenten

4

Edukt 2

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

Produkt 1

HCID 103755472-Chloro-5-ethyl-6-methyl-3-nitropyridineAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-3861344d06fa41ed90f224e026380e4b
Quelldatensatz
uspto-grants-1994_05
Patentnummer
US05308854

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