Reaktion #51891

ord-07aa7eaef78e44df9ce345f34b349766

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solution was partitioned between EtOAc (120 ml) and HCl (50 ml, 0.4 M)
  2. 2
    Waschenthe aqueous layer washed with EtOAc (3×25 ml)
  3. 3
    Trocknenthe combined organic layers dried (MgSO4)
  4. 4
    Sonstigeevaporated to dryness
  5. 5
    SonstigeThe residue was recrystallized from EtOAc

Vorschrift

A solution of the 3-trifluoromethyl-4-[bis(2-hydroxyethyl) amino]benzonitrile and NaOH (0.8 g, 0.02 mol) in aqueous ethanol (10 ml, 50%) was refluxed for 2 hours. The solution was partitioned between EtOAc (120 ml) and HCl (50 ml, 0.4 M), the aqueous layer washed with EtOAc (3×25 ml), the combined organic layers dried (MgSO4) and evaporated to dryness. The residue was recrystallized from EtOAc to give 0.39 g of white crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06852755B1uspto-grants-2005_02