反応 #158376

ord-167c0433bb7b4fd3bad45165816e7d1b

溶媒

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to room temperature
  2. 2
    その他The organic layer was separated
  3. 3
    洗浄washed with water and saturated brine
  4. 4
    乾燥dried over anhydrous magnesium sulfate
  5. 5
    その他the solvent was evaporated under reduced pressure
  6. 6
    その他The residue was purified by silica gel column chromatography (ethyl acetate/hexane)

実験手順

A mixture of methyl 4-fluoro-3-methoxybenzoate (2.13 g), 4-bromo-1H-imidazole (3.74 g) and potassium carbonate (4.80 g) in DMF (20 mL) was stirred at 100° C. overnight, and allowed to cool to room temperature, and ethyl acetate and water were added. The organic layer was separated, washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (0.580 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08822699B2uspto-grants-2014_09