反応 #73904

ord-d1a8431d8cb34cfeb130d26feef503b6

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The organic phase was separated
  2. 2
    洗浄washed with brine
  3. 3
    乾燥dried over anhydrous MgSO4
  4. 4
    その他The solvent was evaporated under reduced pressure at room temperature
  5. 5
    洗浄eluted with diethyl ether

実験手順

5-Bromobenzofuran-2-carboxylic acid (4.68 g) was suspended in carbon tetrachloride (150 ml) and water (50 ml). To this was added sodium bicarbonate (3.36 g), followed by Selectflor (7.1 g) and the reaction mixture was stirred rapidly for 20 hours. The reaction mixture was diluted with dichloromethane and 2N sodium hydroxide solution. The organic phase was separated, washed with brine and dried over anhydrous MgSO4. The solvent was evaporated under reduced pressure at room temperature. The residue was applied to a silica cartridge (20 g) and eluted with diethyl ether. This gave 5-bromo-2-fluoro-1-benzofuran (1.4 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541579B2uspto-grants-2013_09