Reaktion #41791

ord-6c3a22c870d246fbbefe33def8efab1f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeflushed with nitrogen
  2. 2
    SonstigeHydrogen was flushed through the reaction for 1-2 hours or until the reaction
  3. 3
    SonstigeNitrogen was flushed through the reaction for 15 minutes before the reaction
  4. 4
    Filtrationwas filtered through a celite pad
  5. 5
    WaschenThe celite pad was washed with excess methanol before it
  6. 6
    Sonstigeall removed by evaporation under reduced pressure

Vorschrift

A solution of 4-(4-methylamino-3-nitro-phenoxy)-pyridine-2-carboxylic acid (2-hydroxy-ethyl)-amide (1 eq) and 10% palladium on carbon (0.1 eq) in methanol was stirred at room temperature and flushed with nitrogen. Hydrogen was flushed through the reaction for 1-2 hours or until the reaction was determined to be complete by HPLC. Nitrogen was flushed through the reaction for 15 minutes before the reaction was filtered through a celite pad. The celite pad was washed with excess methanol before it was all removed by evaporation under reduced pressure to afford the product as a light yellow solid. LCMS m/z 303.2 (MH+), tR=1.5 min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728010B2uspto-grants-2010_06