Reaktion #83535

ord-e2e957f3b549479c94a5f8e24c545d13

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture is filtered
  2. 2
    Waschenthe filter residue is washed with dichloromethane
  3. 3
    Einengenthe filtrate is concentrated by evaporation
  4. 4
    Sonstigethe residue is chromatographed on silica gel with hexane/10-20% ethyl acetate

Vorschrift

152.6 g of potassium carbonate and 15.3 g of cesium carbonate are added to a solution of 122 g of 3-hydroxy-2-iodopyridine and 65.7 ml of benzyl bromide in 1.5 l of dimethylformamide, and the suspension is stirred under argon atmosphere for 20 hours at room temperature. The reaction mixture is filtered, the filter residue is washed with dichloromethane, the filtrate is concentrated by evaporation, and the residue is chromatographed on silica gel with hexane/10-20% ethyl acetate. 146.3 g of 3-benzyloxy-2-iodopyridine is obtained as oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05624943uspto-grants-1997_04