Phosphorus oxychloride → 2-Chloroisonicotinic acid

HRID 2738

Reaktionsgleichung

Reaktionsgleichung von HRID 2738
P(Cl)(Cl)([Cl:3])=O.[C:6]([OH:15])(=[O:14])[C:7]1[CH:12]=[CH:11][N+:10]([O-])=[CH:9][CH:8]=1>>[Cl:3][C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][N:10]=1)[C:6]([OH:15])=[O:14]

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 261304-Pyridinecarboxylic acid, 1-oxide

Produkt 1

HCID 2369852-Chloroisonicotinic acid

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

Phosphorus oxychloride (220.7 g) was added to isonicotinic acid N-oxide (50.064 g), and the mixture was stirred on an oil bath at 120° C. for 7 hours. The reaction mixture was slowly poured into ice water with vigorously stirring to precipitate light yellow crystals. The mixture was adjusted to approximately pH 4 with 4N NaOH aqueous solution. The resulting crystals were filtered out, washed with water, and dried by vacuum heating (60° C.) to obtain the above-captioned compound ([9]-(92)-467) (37.845 g).

Aufarbeitung

  1. stirringwith vigorously stirring
  2. customto precipitate light yellow crystals
  3. filtrationThe resulting crystals were filtered out
  4. washwashed with water
  5. customdried by vacuum
  6. temperatureheating (60° C.)
  7. customto obtain the above-captioned compound ([9]-(92)-467) (37.845 g)

Quellen und Nachweise

ORD-Eintrag
ord-8debf37587f1426b9a2fd8782e5c9316
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05731310

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