Reaktion #444800

ord-19b772d06da04a619963f3670bb5fa35

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis heated
  2. 2
    Temperaturunder reflux for 22 hours
  3. 3
    FiltrationFiltration of the hot reaction mixture
  4. 4
    Waschenwashing of the crystallizate with isopropanol and diethyl ether
  5. 5
    Sonstigedrying under a high vacuum

Vorschrift

A mixture of 0.837 g (4.079 mmol) of 4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-one oxime, 0.40 g (4.077 mmol) of 1,2-diamino-imidazole, 23 ml of isopropanol and 1.33 ml of concentrated hydrochloric acid is heated under reflux for 22 hours. Filtration of the hot reaction mixture, washing of the crystallizate with isopropanol and diethyl ether and drying under a high vacuum yield the title compound, m.p. 258°-260° C. (decomp.), 1H-NMR (DMSO/D2O): δ=8.29 (d, 1H); 7.80 (d, 1H); 7.65 (t, 1H); 7.55 (d, 1H); 7.13 (d, 1H); 3.22-3.32 (m 4H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05840911uspto-grants-1998_11