Reaktion #40585

ord-27352282c0af4dfbb16addeee00b36b0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeis prepared
  2. 2
    workup.STIRRINGThe reaction mixture is kept stirring for 30 minutes, at room temperature
  3. 3
    SonstigeThe aqueous phase obtained
  4. 4
    Extraktionis extracted twice with ethyl acetate
  5. 5
    TrocknenThe combined organic phases are dried over magnesium sulfate
  6. 6
    Einengenconcentrated under reduced pressure

Vorschrift

A mixture of 1.83 g (14.7 mM) of 5-amino-2-methoxypyridine and 1.21 g (14.7 mM) of sodium acetate in 12 ml of acetic acid is prepared and 0.75 ml (14.7 mM) of bromine is added gently, with stirring and while maintaining at room temperature. The reaction mixture is kept stirring for 30 minutes, at room temperature, and 200 ml of saturated sodium thiosulfate solution are then added. The aqueous phase obtained is extracted twice with ethyl acetate. The combined organic phases are dried over magnesium sulfate and concentrated under reduced pressure. 3 g of the expected compound are obtained in the form of a violet-colored solid (quantitative yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728002B2uspto-grants-2010_06