Formic Acid → 5-Formamido-1-methylpyrazole

HRID 1031195Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1031195
C(O[C:5](=[O:7])C)(=O)C.C(O)=O.[NH2:11][C:12]1[N:16]([CH3:17])[N:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C.O>[CH:5]([NH:11][C:12]1[N:16]([CH3:17])[N:15]=[CH:14][CH:13]=1)=[O:7]

Komponenten

7

Edukt 4

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 1369272-Methyl-2H-pyrazol-3-ylamine

Produkt 1

HCID 27558695-Formamido-1-methylpyrazole

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

A mixture of acetic anhydride (38.86 ml) and formic acid (15.54 ml) was stirred at 45° C. for 45 minutes. To this mixture was added 5-amino-1-methylpyrazole (10 g) under ice-cooling, and the reaction mixture was stirred at the same temperature for 10 minutes. The resultant mixture was poured into a mixture of water and ethyl acetate, and the resultant solution was adjusted to pH 8 with potassium carbonate. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate six times. The organic layers were combined, dried over magnesium sulfate, and evaporated in vacuo to give 5-formamido-1-methylpyrazole (12.88 g).

Aufarbeitung

  1. temperaturecooling
  2. stirringthe reaction mixture was stirred at the same temperature for 10 minutes
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with ethyl acetate six times
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a0c94160acef4da5b829a5e276ddc493
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05108997

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