反応 #2314287

ord-ddc232abfd544438b4acbac4d5921aaa

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONis added
  2. 2
    抽出extracted with ethyl acetate
  3. 3
    洗浄The combined organic layers are washed with brine
  4. 4
    乾燥dried over magnesium sulfate
  5. 5
    濃縮The solution is concentrated in vacuo

実験手順

To a solution of 3-(4-hydroxyphenyl)-1-propanol 3A (4.0 g) and tripohenylphosphine (7.96 g) in anhydrous dichloromethane (77 mL), cooled to 0° C., is added, dropwise, a solution of tetrabromomethane (9.59 g) in anhydrous dichloromethane (15.4 mL). The reaction mixture gradually warmed to room temperature and allowed to stir overnight. The solution is then poured into water and extracted with ethyl acetate. The combined organic layers are washed with brine and dried over magnesium sulfate. The solution is concentrated in vacuo.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06413448B1uspto-grants-2002_07