Nitric Acid → 2,5-Dichloro-4-nitro-1-oxo-1lambda~5~-pyridine

HRID 1988757Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1988757
OS(O)(=O)=O.O=S(=O)=O.[N+:10]([O-:13])(O)=[O:11].[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][N+:16]=1[O-:22]>OS(O)(=O)=O>[Cl:14][C:15]1[CH:20]=[C:19]([N+:10]([O-:13])=[O:11])[C:18]([Cl:21])=[CH:17][N+:16]=1[O-:22]

Komponenten

5

Edukt 3

HCID 944Nitric AcidHCID 24681Fuming sulfuric acidHCID 113326572,5-Dichloro-pyridine 1-oxide

Produkt 1

HCID 222840452,5-Dichloro-4-nitro-1-oxo-1lambda~5~-pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

At 0° C., 30% oleum (13 mL) is added slowly to fuming HNO3 (22 mL) and the resulting mixture is added slowly to the solution of 2,5-dichloro-pyridine 1-oxide (5.2 g, 31 mmol) in concentrated H2SO4. After addition, the reaction mixture is warmed to room temperature over 1 hr, then heated to 80° C. for 2 hr. After cooling to room temperature, the mixture is poured into ice (120 g) and precipitate is formed gradually. The solid is collected by filtration and washed with water. The product is obtained as yellow solid. 1H NMR (CDCl3) δ 8.46 (s, 1H), 8.25 (s, 1).

Aufarbeitung

  1. additionAfter addition
  2. temperatureheated to 80° C. for 2 hr
  3. temperatureAfter cooling to room temperature
  4. customprecipitate is formed gradually
  5. filtrationThe solid is collected by filtration
  6. washwashed with water
  7. customThe product is obtained as yellow solid

Quellen und Nachweise

ORD-Eintrag
ord-718fa53d733b46748fda9ac507d1a4dc
Quelldatensatz
uspto-grants-2010_01
Patentnummer
US07642267B2

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