反応 #8495

ord-4debe123c0e647088929ba120d5af46f

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated to 190 C for 69 h
  2. 2
    温度to cool
  3. 3
    抽出This mixture was extracted with CHCl3 (1×100 mL)
  4. 4
    洗浄the organic layer was then washed with H2O (2×50 mL)
  5. 5
    乾燥The organic layer was dried (anh. Na2SO4)
  6. 6
    その他rotary evaporated (90° C.)

実験手順

A mixture of 2-[2-(4-fluorophenyl)ethyl]benzonitrile (8.03 g, 35.6 mmol, 1 equiv) and aq. NaOH (10N; 16 mL, 160 mmol, 4.5 equiv) in ethylene glycol (100 mL) was heated to 190 C for 69 h. After allowing the reaction mixture to cool, H2O (300 mL) was added, followed by 12N HCl (16 mL). This mixture was extracted with CHCl3 (1×100 mL) and the organic layer was then washed with H2O (2×50 mL). The organic layer was dried (anh. Na2SO4) and rotary evaporated (90° C.). This provided 7.44 g (85.4%) of a light-yellow solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087765B2uspto-grants-2006_08