反応 #70445

ord-c8a0a158050e49dcaf45dfee4187d4a0

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate
  2. 2
    洗浄The organic layer was washed with brine
  3. 3
    乾燥dried over anhydrous sodium sulfate
  4. 4
    濃縮concentrated under reduced pressure
  5. 5
    その他The residue was purified by silica gel column chromatography (hexane/ethyl acetate=19/1→3/2)

実験手順

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%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08536176B2uspto-grants-2013_09