Ammonium Acetate → HCID 68677556, Verbindung

HRID 2233016Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2233016
C([O:3][C:4]([C:6]1[N:10]([CH2:11][C:12](=O)[C:13]([CH3:16])([CH3:15])[CH3:14])[C:9](=[O:18])[N:8]([C:19]([CH3:22])([CH3:21])[CH3:20])[N:7]=1)=O)C.C([O-])(=O)C.[NH4+:27]>CO>[C:19]([N:8]1[C:9](=[O:18])[N:10]2[CH:11]=[C:12]([C:13]([CH3:16])([CH3:15])[CH3:14])[NH:27][C:4](=[O:3])[C:6]2=[N:7]1)([CH3:22])([CH3:21])[CH3:20]

Komponenten

4

Edukt 2

HCID 517165Ammonium AcetateHCID 68675630HCID 68675630, Verbindung

Produkt 1

HCID 68677556HCID 68677556, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 8.60 g of the product of Step C and 21.30 g of ammonium acetate in MeOH was heated in a sealed system at 100° C. for 24 h. The solution was cooled to ambient temperature and concentrated to leave an oil that was partitioned between EtOAc and water. The aqueous layer was acidified to pH 5 with concentrated HCl and then extracted with EtOAc. The combined organic layers were washed with sat. sodium chloride, dried over sodium sulfate, filtered, and concentrated to provide 2,6-di-tert-butyl-2H,7H-[1,2,4]triazolo[4,3-a]pyrazine-3,8-dione as a white solid. MS (M+H+)=265.3.

Aufarbeitung

  1. concentrationconcentrated
  2. customto leave an oil that
  3. customwas partitioned between EtOAc and water
  4. extractionextracted with EtOAc
  5. washThe combined organic layers were washed with sat. sodium chloride
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-256a1cf901e64a268c09b48ce576c220
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07709473B2

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