Nitric Acid → 2,6-Dichloro-4-nitropyridine

HRID 1190811Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1190811
[N+:1]([O-:4])(O)=[O:2].[Cl:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([Cl:12])[N+:7]=1[O-].[N+]([O-])=O.O.N>S(=O)(=O)(O)O>[Cl:5][C:6]1[CH:11]=[C:10]([N+:1]([O-:4])=[O:2])[CH:9]=[C:8]([Cl:12])[N:7]=1

Komponenten

6

Edukt 4

HCID 944Nitric AcidHCID 8176732,6-Dichloropyridine N-OxideHCID 12896473Azane;hydrateHCID 178526396Nitrogen Dioxide

Produkt 1

HCID 38410702,6-Dichloro-4-nitropyridineAusbeute 66,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

To a solution of 95% concentrated nitric acid (21 mL) and 98% concentrated sulfuric acid (50 mL) was added 2,6-dichloropyridine-N-oxide (12.8 g, 78 mmol). After the reaction was performed at 148° C. by stirring for 1 h, it was continued when the temperature was increased to 156° C. until no nitrogen dioxide was released. The reaction solution was cooled to room temperature, poured into 150 g ice water, and adjusted to pH=6 with ammonia water to precipitate a solid product. It was subjected to suction filtration. The resultant crude product was recrystallized with petroleum ether to afford 10 g yellow solid with a yield of 66.4%.

Aufarbeitung

  1. customwas performed at 148° C.
  2. customto precipitate a solid product
  3. filtrationIt was subjected to suction filtration
  4. customThe resultant crude product was recrystallized with petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-9a85f4ef23f641f78018d99292fafc80
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08680089B2

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