反応 #365505

ord-dd051cc541b3438c97c876251a083e4f

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度to reflux for 18 hours
  3. 3
    温度to cool
  4. 4
    ろ過the potassium salts were filtered
  5. 5
    濃縮concentrated
  6. 6
    抽出The residue was extracted with chloroform
  7. 7
    洗浄washed with H2O
  8. 8
    乾燥dried over sodium sulfate
  9. 9
    濃縮concentrated

実験手順

3-{[4-(2-Butynyloxy)phenyl]sulfonyl}-3-piperidinecarboxylate hydrogen chloride (2.97 g, 8.0 mmol), ethyl iodide (1.28 g, 8 mmol) and dry powdered potassium carbonate (3.8 g) in dry acetone (60 ml) was heated to reflux for 18 hours. The mixture was allowed to cool and the potassium salts were filtered and concentrated. The residue was extracted with chloroform and washed with H2O, dried over sodium sulfate and concentrated to afford ethyl 3-{[4-(2-butynyloxy)phenyl]sulfonyl}-1-ethyl-3-piperidinecarboxylate. This product was used without further purification. Amber gum, yield 3.47 g (99%); MS (ES): m/z 394 (M+H)+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06358980B1uspto-grants-2002_03