Reaktion #92418

ord-03170a056cb542a887399f8eb3dd5118

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationfiltered
  2. 2
    workup.ADDITIONThe filtrate was diluted with water
  3. 3
    Extraktionextracted as in Example 1(d)
  4. 4
    workup.DISTILLATIONThe solvent was distilled off

Vorschrift

To a solution of the compound of Example 155(c) N-(3-(4-bromo-2-nitro-phenylamino)-5-(1H-1,2,4-triazol-1-yl)phenyl)acetamide (5.2 g, 12.5 mmol) in ethanol (100 ml) were added calcium chloride (2.78 g, 25 mmol, 2 eq.) and iron powder (1.3 g, 25 mmol, 2 eq.) and the mixture was heated at 100° C. for 4 h and filtered. The filtrate was diluted with water and extracted as in Example 1(d). The solvent was distilled off and the crude residue was directly used for the next step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447091B2uspto-grants-2016_09