Ethyl Acetoacetate → HCID 178429414, Verbindung

HRID 24963

Reaktionsgleichung

Reaktionsgleichung von HRID 24963
C(=O)(O)O.[NH2:5][C:6]([NH2:8])=[NH:7].[C:9](OCC)(=[O:14])[CH2:10][C:11]([CH3:13])=O>C(O)C>[CH3:13][C:11]1[NH:5][C:6]([NH2:8])=[N:7][C:9](=[O:14])[CH:10]=1

Komponenten

4

Edukt 2

HCID 8868Ethyl AcetoacetateHCID 286947Carbonic acid-guanidine (1:1)

Produkt 1

HCID 178429414HCID 178429414, VerbindungAusbeute 125,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperatureThe reaction solution was gradually heated
  2. temperatureto reflux temperature
  3. customEthanol (300 mL) was evaporated
  4. temperaturethe reaction mixture was heated
  5. temperatureunder reflux for two hours
  6. temperatureAfter the reaction mixture was cooled
  7. addition300 mL of hexane was added
  8. filtrationThe resulting precipitate was filtered
  9. washwashed
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d0a2792311094e53ba927cdb4a416d7a
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06858359B2

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