Ethanol → HCID 178418578, Verbindung

HRID 5201Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 5201
[C:1]([O-:7])(=[O:6])[CH2:2][C:3]([CH3:5])=O.[Li+].[C:9]([NH:12][NH2:13])([NH2:11])=[NH:10].Cl.C(O)C>O>[C:9]([NH:12][N:13]=[C:3]([CH3:5])[CH2:2][C:1]([OH:7])=[O:6])(=[NH:10])[NH2:11]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 27242463-oxobutanoic acid lithium saltHCID 178418668HCID 178418668, Verbindung

Produkt 1

HCID 178418578HCID 178418578, VerbindungAusbeute 54,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

Lithium acetoacetate (0.655 g) in 2 ml water treated with 0.665 g aminoguanidine HCl in 1.33 ml water. The solution was heated to reflux over 30 minutes and then allowed to cool. Ethanol (10 ml) was added and the mixture was stored at -20° C. for 24 hrs., then at 4° C. for 24 hrs. The mixture was allowed to reach room temperature and filtered. The filtrate was concentrated to a paste and triturated with 5 ml ethanol. Filtration and washing with ethanol gave 0.522 g of the hydrazone as a microcrystalline powder, melting point 138.6°-140° C.

Aufarbeitung

  1. temperatureThe solution was heated
  2. temperatureto reflux over 30 minutes
  3. temperatureto cool
  4. wait, then at 4° C. for 24 hrs
  5. customto reach room temperature
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated to a paste
  8. customtriturated with 5 ml ethanol
  9. filtrationFiltration
  10. washwashing with ethanol

Quellen und Nachweise

ORD-Eintrag
ord-765eee938f5f4e1793095537f302f9ea
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05243071

Notizen zur Reaktion

Wird geladen…