Reaktion #53241

ord-d0a2792311094e53ba927cdb4a416d7a

Reaktionsgleichung

N=C(N)N.O=C(O)O
guanidine carbonate
CCOC(=O)CC(C)=O
ethyl acetoacetate
Cc1cc(=O)nc(N)[nH]1
6-methyl-iso cytosine
Ausbeute 125.6%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction solution was gradually heated
  2. 2
    Temperaturto reflux temperature
  3. 3
    SonstigeEthanol (300 mL) was evaporated
  4. 4
    Temperaturthe reaction mixture was heated
  5. 5
    Temperaturunder reflux for two hours
  6. 6
    TemperaturAfter the reaction mixture was cooled
  7. 7
    workup.ADDITION300 mL of hexane was added
  8. 8
    FiltrationThe resulting precipitate was filtered
  9. 9
    Waschenwashed
  10. 10
    Sonstigedried

Vorschrift

Dry ethanol (600 mL), 91.89 g of guanidine carbonate, and 146.1 g of ethyl acetoacetate were added to a 1 L flask. The reaction solution was gradually heated to reflux temperature and stirred overnight. Ethanol (300 mL) was evaporated, and the reaction mixture was heated under reflux for two hours. After the reaction mixture was cooled, 300 mL of hexane was added. The resulting precipitate was filtered, washed and dried. 119.3 g of 6-methyl-iso cytosine was obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858359B2uspto-grants-2005_02