Reaktion #306616

ord-2ffb4caf7fc94b52b872d07727e45400

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction solution was concentrated in vacuo, 20 ml of chloroform
  2. 2
    workup.ADDITIONwas added to the resulting residue
  3. 3
    Einengenthe mixture was again concentrated in vacuo
  4. 4
    Sonstigethe residue from which the pyridine had been removed
  5. 5
    Sonstigewas purified by silica gel column chromatography

Vorschrift

2-Amino-3-nitrophenol (308 mg) was dissolved in 10 ml of pyridine, then 341 mg of 4-methoxybenzoyl chloride was added at 0° C. and the mixture was stirred at room temperature for 18 hours. The reaction solution was concentrated in vacuo, 20 ml of chloroform was added to the resulting residue and the mixture was again concentrated in vacuo. This operation was further repeated three times, and the residue from which the pyridine had been removed was purified by silica gel column chromatography using chloroform as an eluting solvent to give 428 mg of 2′-hydroxy-4-methoxy-6′-nitrobenzanilide.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: USRE043481E1uspto-grants-2012_06