Reaktion #70445

ord-c8a0a158050e49dcaf45dfee4187d4a0

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ethyl acetate
  2. 2
    WaschenThe organic layer was washed with brine
  3. 3
    Trocknendried over anhydrous sodium sulfate
  4. 4
    Einengenconcentrated under reduced pressure
  5. 5
    SonstigeThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=19/1→3/2)

Vorschrift

To a solution of 2,5-dibromopyridin-3-ol (200 mg, 0.791 mmol) in dry N,N-dimethylformamide (8 mL) was added potassium carbonate (164 mg, 1.19 mmol) and benzyl bromide (0.11 mL, 0.949 mmol). The mixture was stirred at room temperature for 2 hours, diluted with water (10 mL) and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=19/1→3/2) to give the title compound as a white crystal (211 mg, yield 78%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536176B2uspto-grants-2013_09