Reaktion #65789

ord-a0ae2db61f414b338b9f80a607d7bf72

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was heated
  2. 2
    Temperaturunder reflux for 20 minutes
  3. 3
    EinengenAfter the reaction mixture was concentrated to dryness

Vorschrift

A mixture of 0.34 g of 3,4-diethoxycarbonyl-3-nitro-2-phenyl-6-sulfopyridine, 0.41 g of reduced iron and 7 ml of ethanol was heated to 60° C., and then 0.5 ml of conc. hydrochloric acid was added. The mixture was heated under reflux for 20 minutes. After the reaction mixture was concentrated to dryness, the residue was subjected to silica gel column chromatography (eluent:chloroform/methanol 5:1), to give 0.24 g of the title compound as pale yellow crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05420275uspto-grants-1995_05