Acetic Anhydride → HCID 178474341, Verbindung

HRID 522598Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 522598
[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 %

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 was then added dropwise and the resulting suspension was heated at reflux overnight. Then, the mixture was allowed to cool down to room temperature and the solid obtained was filtered off and characterized as the title compound (8.4 g, 0.067 mol, 49% yield). After concentration of the filtrate, a second precipitate was obtained (2.7 g, 0.021 mol, 16% yield), 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-782ec822d4d44fa4a0eb22f6171b8890
Quelldatensatz
uspto-grants-2016_05
Patentnummer
US09334265B2

Notizen zur Reaktion

Wird geladen…