反応 #76447

ord-cda7c95d3a9d45f4a7273c50490ba941

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Most of the solvent was removed in vacuo
  2. 2
    その他the residue was partitioned between diethyl ether and water
  3. 3
    洗浄The organic phase was washed with saturated aqueous sodium bicarbonate solution and brine
  4. 4
    乾燥dried over anhydrous magnesium sulfate
  5. 5
    ろ過filtered
  6. 6
    その他the filtrate was evaporated in vacuo

実験手順

4-Fluoro-3-nitrophenylacetic acid (31.0 g, 0.156 mol) was added to a mixture of concentrated sulfuric acid (1.6 ml) and methanol (160 ml) and the mixture was stirred for 3 days at room temperature. Most of the solvent was removed in vacuo and the residue was partitioned between diethyl ether and water. The organic phase was washed with saturated aqueous sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate, filtered and the filtrate was evaporated in vacuo to give methyl 4-fluoro-3-nitrophenylacetate (27.2 g) as a yellow oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06703347B2uspto-grants-2004_03