Reaktion #640531

ord-57cb82a95d384ee4b75e6f8e4bb38f56

Reaktionsgleichung

Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)c([N+](=O)[O-])c1
4-[1-(4-chloro-3-nitrophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine
Nc1cc(C(=O)Cn2c(-c3nonc3N)nc3ccccc32)ccc1Cl
title compound
Nc1cc(C(=O)Cn2c(-c3nonc3N)nc3ccccc32)ccc1Cl
4-[1-(3-Amino-4-chlorophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationFiltration and evaporation at reduced pressure
  2. 2
    Sonstigegives the crude product
  3. 3
    SonstigePurification
  4. 4
    Extraktionby extraction with ethyl acetate and chromatography on silicagel

Vorschrift

To a stirred solution of 4-[1-(4-chloro-3-nitrophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine (0.07 g, 0.175 mmol) in ethanol (6 ml) and water (1 ml) is added two drops of concentrated hydrochloric acid and iron powder (0.1 g, 17.5 mmol). The reaction mixture is heated at 80° C. for 8 hours. Filtration and evaporation at reduced pressure gives the crude product. Purification by extraction with ethyl acetate and chromatography on silicagel yields the title compound as colorless solid, m.p. 228-230° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: USRE042890E1uspto-grants-2011_11