Nitric Acid → 5-Chloro-1,3-dimethyl-4-nitro-1H-pyrazole

HRID 1031336

Reaktionsgleichung

Reaktionsgleichung von HRID 1031336
OS(O)(=O)=O.[Cl:6][C:7]1[N:11]([CH3:12])[N:10]=[C:9]([CH3:13])[CH:8]=1.[N+:14]([O-])([OH:16])=[O:15]>>[Cl:6][C:7]1[N:11]([CH3:12])[N:10]=[C:9]([CH3:13])[C:8]=1[N+:14]([O-:16])=[O:15]

Komponenten

4

Edukt 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 5215075-Chloro-1,3-dimethylpyrazole

Produkt 1

HCID 2795155-Chloro-1,3-dimethyl-4-nitro-1H-pyrazole

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

Concentrated H2SO4 (35 g) was added to 10 ml of 90% HNO3 and at 75°-85° C., 13 g (0.1 mol) of 5-chloro-1,3-dimethylpyrazole was added dropwise with stirring to maintain the temperature at 85° C. After completion of the addition, the mixture was heated at 75 -85° C. for 1.5 hr. The nitration mixture was cooled and poured into ice. The suspension was filtered and the solid was washed with water and dried to give 14.5 g of the title compound. m.p. 70° C.

Aufarbeitung

  1. additionAfter completion of the addition
  2. temperaturethe mixture was heated at 75 -85° C. for 1.5 hr
  3. temperatureThe nitration mixture was cooled
  4. additionpoured into ice
  5. filtrationThe suspension was filtered
  6. washthe solid was washed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-cd7d66b7bcbb4b85af610717808f9306
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04954164

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