Reaktion #689620

ord-f27acf8f24c948bdabc50eece916231a

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    WaschenThe mixture was washed with water, aqueous 4% sodium bicarbonate, brine
  3. 3
    Trocknendried over sodium sulphate
  4. 4
    Sonstigethe solvent removed under reduced pressure
  5. 5
    SonstigeThe residue was purified by column chromatography on silica flash

Vorschrift

To an ice-cooled solution of 3-aminopyridine (6 g, 63.8 mmol) and triethylamine (9.72 mL, 70.2 mmol) in 124 mL of dichloromethane under argon, was carefully added pivaloyl chloride (7.92 mL, 64.4 mmol) in 16 mL of dichloromethane. After the addition was completed, the reaction mixture was stirred at 0° C. for 15 minutes and at room temperature for 18 hours. The mixture was washed with water, aqueous 4% sodium bicarbonate, brine, dried over sodium sulphate and the solvent removed under reduced pressure. The residue was purified by column chromatography on silica flash, using hexane/ethyl acetate (85:15) as eluents, to yield the title compound (8.5 g, 75%) as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07906530B2uspto-grants-2011_03