Reaktion #52679

ord-72dacf05edc84f9095ba6d710f037b89

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solids were removed by filtration
  2. 2
    Sonstigethe solvent evaporated
  3. 3
    workup.ADDITIONThe residue was treated with ethyl acetate
  4. 4
    workup.ADDITIONThe ethyl acetate solution containing insoluble solid
  5. 5
    SonstigeThe collected ethyl acetate solution was evaporated
  6. 6
    Sonstigethe residue dried under vacuum

Vorschrift

Zinc dust (6.5 g) was added to a solution of 3,3-dibromo-7-azaoxindole (2.9 g) in acetic acid (20 ml) and acetonitrile (30 ml). The mixture was stirred for 2 hours at room temperature. The solids were removed by filtration and the solvent evaporated. The residue was treated with ethyl acetate. The ethyl acetate solution containing insoluble solid was passed through a short column of silica gel. The collected ethyl acetate solution was evaporated and the residue dried under vacuum to give 1.8 g (91% yield) of 7-aza-2-oxindole acetic acid salt.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06855730B2uspto-grants-2005_02