Acetic Anhydride → HCID 178474341, Verbindung

HRID 38672Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 38672
[NH:1]1[CH:5]=[CH:4][C:3]([NH2:6])=[N:2]1.C([O-])(O)=O.[Na+].[C:12](OC(=O)C)(=[O:14])[CH3:13]>O>[NH:1]1[CH:5]=[CH:4][C:3]([NH:6][C:12](=[O:14])[CH3:13])=[N:2]1

Komponenten

5

Edukt 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 178418806HCID 178418806, Verbindung

Produkt 1

HCID 178474341HCID 178474341, VerbindungAusbeute 49,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

1H-pyrazol-3-amine (ALDRICH, 11.32 g, 0.136 mol) was dissolved in 100 mL of distilled water. NaHCO3 (34 g, 0.408 mol) was slowly added. Acetic anhydride (27.55 g, 0.272 mol) was then added dropwise and the resulting suspension was heated at reflux overnight. Then, the mixture was allowed to cool down to r.t. and the solid obtained was filtered off and characterized as the title compound (8.4 g, 0.067 mol, 49%). After concentration of the filtrate, a second precipitate was obtained (2.7 g, 0.021 mol, 16%), also characterized as the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm: 12.23 (br s, 1H), 10.30 (br s, 1H), 7.55 (br s, 1H), 6.45 (br s, 1H), 1.97 (s, 3H). [ES+MS] m/z 126 (MH+).

Aufarbeitung

  1. temperaturethe resulting suspension was heated
  2. temperatureat reflux overnight
  3. customthe solid obtained
  4. filtrationwas filtered off

Quellen und Nachweise

ORD-Eintrag
ord-2e273e05783d458eb9aeaf2f9b579303
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524750B2

Notizen zur Reaktion

Wird geladen…