Reaktion #46491

ord-2e662f4c81be498890476a80b9eb7a1f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux for 12 hrs
  3. 3
    Temperaturduring heating
  4. 4
    TemperaturThe reaction mixture was cooled
  5. 5
    Sonstigea crystalline precipitate formed
  6. 6
    FiltrationThis was filtered
  7. 7
    Waschenwashed with ethyl acetate and air
  8. 8
    Sonstigedried

Vorschrift

A suspension of 2-amino-5-bromo-3-(hydroxymethyl)pyridine hydrobromide (289 g, 1.02 mole) in 48% aqueous HBr (2.9 L) was heated at reflux for 12 hrs. Complete solution occurred during heating. The reaction mixture was cooled and a crystalline precipitate formed. This was filtered and washed with ethyl acetate and air dried to give the title compound (305 g, 86%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741339B2uspto-grants-2010_06