Potassium Iodide → 1,3-dimethyl-4-nitro-1H-pyrazole-5-carbonitrile

HRID 979052

Reaktionsgleichung

Reaktionsgleichung von HRID 979052
[CH3:1][N:2]1[C:6](Cl)=[C:5]([N+:8]([O-:10])=[O:9])[C:4]([CH3:11])=[N:3]1.[C-]#N.[K+].[I-].[K+].[CH3:17][N:18](C=O)C>C(#N)C>[CH3:1][N:2]1[C:6]([C:17]#[N:18])=[C:5]([N+:8]([O-:10])=[O:9])[C:4]([CH3:11])=[N:3]1

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 6228DimethylformamideHCID 9032Potassium CyanideHCID 2795155-Chloro-1,3-dimethyl-4-nitro-1H-pyrazole

Produkt 1

HCID 965071,3-dimethyl-4-nitro-1H-pyrazole-5-carbonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Fifty-five g of 1,3-dimethyl-4-nitro-5-chloropyrazole was dissolved in 400 ml acetonitrile and 17.45 g potassium cyanide added, followed by 0.5 g potassium iodide and 5 ml DMF. The mixture was refluxed for 22 hours, then cooled, and filtered. The filtrate was concentrated under reduced pressure, then added to stirred water. The resulting percipitate was collected, dried, and recyrstallized in isopropanol. mp, 85°-87° C. A second recrystallization again in ethanol gave the product having increased purity, mp 96°-98° C.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 22 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. additionadded
  6. customThe resulting percipitate was collected
  7. customdried
  8. custommp, 85°-87° C
  9. customA second recrystallization again in ethanol
  10. customgave the product
  11. temperaturehaving increased purity, mp 96°-98° C.

Quellen und Nachweise

ORD-Eintrag
ord-02e5eba2d86747a6ad61fc9c271d97c8
Quelldatensatz
uspto-grants-1987_05
Patentnummer
US04666908

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