Reaktion #1447098

ord-eeed7cb84df54cc28056c5c5beb05544

Reaktionsgleichung

Cl
hydrochloric acid
CCc1ccc(Cc2cc(Br)c(OC)cc2NC(C)=O)cc1
N-[4-bromo-2-(4-ethyl-benzyl)-5-methoxy-phenyl]-acetamide
CCc1ccc(Cc2cc(Br)c(OC)cc2N)cc1
title compound
CCc1ccc(Cc2cc(Br)c(OC)cc2N)cc1
4-Bromo-2-(4-ethyl-benzyl)-5-methoxy-phenylamine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe solution is heated
  2. 2
    Temperaturat reflux temperature for 8 h
  3. 3
    Einengenconcentrated under reduced pressure
  4. 4
    Sonstigeto remove most of the alcohol
  5. 5
    workup.ADDITIONAqueous NaHCO3 solution is added to the rest
  6. 6
    Extraktionthe resulting mixture is extracted twice with ethyl acetate
  7. 7
    WaschenThe combined organic extracts are washed with brine
  8. 8
    Trocknendried (Na2SO4)
  9. 9
    Einengenconcentrated

Vorschrift

Half-concentrated hydrochloric acid (5 mL) is added to a solution of N-[4-bromo-2-(4-ethyl-benzyl)-5-methoxy-phenyl]-acetamide (2.8 g) in isopropanol (20 mL). The solution is heated at reflux temperature for 8 h and then concentrated under reduced pressure to remove most of the alcohol. Aqueous NaHCO3 solution is added to the rest and the resulting mixture is extracted twice with ethyl acetate. The combined organic extracts are washed with brine, dried (Na2SO4) and concentrated to give the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07879806B2uspto-grants-2011_02