Acetic Anhydride → HCID 178474341, Verbindung

HRID 32793Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 32793
[NH2:1][C:2]1[CH:6]=[CH:5][NH:4][N:3]=1.C([O-])(O)=O.[Na+].[CH3:12][C:13](OC(C)=O)=[O:14]>O>[NH:4]1[CH:5]=[CH:6][C:2]([NH:1][C:13](=[O:14])[CH3:12])=[N:3]1

Komponenten

5

Edukt 3

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

Produkt 1

HCID 178474341HCID 178474341, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 3-aminopyrazole (20 g, 0.24 mol) in H2O (36 mL), at 5-10° C., was slowly added NaHCO3 (9.1 g, mol, 3 eq) and then Ac2O (6.79 ml, 2 eq). The reaction mixture was refluxed for 8 hr. It was cooled down to r.t. and was left standing at this temperature for 12 hr to allow crystallization. The white solid was filtered (12.9 g) and the mother liquor volume was reduced. A second batch of white solid (3.4 g) was obtained after crystallization. The two batches were combined to give the title compound (16.3 g, 54%).

Aufarbeitung

  1. customat 5-10° C.
  2. temperatureThe reaction mixture was refluxed for 8 hr
  3. waitwas left
  4. customcrystallization
  5. filtrationThe white solid was filtered (12.9 g)

Quellen und Nachweise

ORD-Eintrag
ord-d8cc33e5f25f40949a2c7f8221c44612
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07427630B2

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