反応 #1144532

ord-366e6e684c544a08bf8344d4e24ece50

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出After extraction with ethyl acetate
  2. 2
    洗浄the organic layer was washed with water
  3. 3
    乾燥brine, dried (MgSO4)
  4. 4
    その他the solvent evaporated
  5. 5
    ろ過The solid was filtered off
  6. 6
    洗浄washed with hexane
  7. 7
    その他dried under vacuum

実験手順

The starting material 5-benzyloxy-2-fluoro-4-methylnitrobenzene was obtained by adding benzyl bromide (3 ml, 25 mmol) to a solution of 2-fluoro-5-hydroxy-4-methylnitrobenzene (3.92 mg, 23 mmol) in DMF (70 ml) containing potassium carbonate (9.5 g, 68 mmol). After stirring for 3 hours at 60° C., the mixture was diluted with water and adjusted to pH2. After extraction with ethyl acetate, the organic layer was washed with water and then brine, dried (MgSO4) and the solvent evaporated. The solid was filtered off, washed with hexane and dried under vacuum to give 5-benzyloxy-2-fluoro-4-methylnitrobenzene (4.83 g, 80%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06514971B1uspto-grants-2003_02