反応 #1624

ord-37aef411031a48079180fe910acb60fa

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The solution was concentrated under reduced pressure and product
  2. 2
    その他dried under in vacuo
  3. 3
    抽出extracted with dichloromethane containing a small proportion of methanol (5×100 ml)
  4. 4
    乾燥The combined organic layers were dried over sodium sulfate
  5. 5
    その他evaporated to dryness

実験手順

4-(2-t-Butoxycarbonylaminoethyl)phenoxymethylphosphonic acid, diethyl ester (2.856 g, 9.95 mMol) in methylene chloride (300 ml) and trifluoracetic acid (16 ml) was stirred at room temperature for 5 h. The solution was concentrated under reduced pressure and product dried under in vacuo. The trifluoacetic acid salt was neutralized with aqueous sodium carbonate and extracted with dichloromethane containing a small proportion of methanol (5×100 ml). The combined organic layers were dried over sodium sulfate and evaporated to dryness to give the title compound as a pale yellow gum.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726165uspto-grants-1998_03