Reaktion #52599

ord-93fe4523593c4d208f99e218af9ad7d3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe solid was filtered from the mixture
  2. 2
    Sonstigethe solvent evaporated
  3. 3
    workup.ADDITIONThe ethyl acetate solution containing insoluble solid
  4. 4
    SonstigeThe collected ethyl acetate solution was evaporated
  5. 5
    Sonstigethe residue dried under vacuum

Vorschrift

3,3-Dibromo-7-azaoxindole (2.9 g) was dissolved in a mixture of 20 mL of acetic acid and 30 mL of acetonitrile. To the solution was added 6.5 g of zinc dust. The mixture was stirred for 2 hrs at room temperature. The solid was filtered from the mixture and the solvent evaporated. The residue was slurried 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 (yield 91%) of 7-azaoxindole acetic acid salt.

Quelle

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