反応 #2892

ord-eb5bfefcbfd94ea0be77c604cb53b9bd

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with dichloromethane
  2. 2
    洗浄The combined extracts were washed with brine
  3. 3
    その他dried
  4. 4
    その他the solvent removed
  5. 5
    その他to leave a brown oil which
  6. 6
    workup.DISTILLATIONwas purified by vacuum distillation, b.p. 70° C. at 2 mbar

実験手順

3-Chloropentane-2,4-dione (46.5 g), propionamide (50 g) and propionic acid (151 g) were heated at 145° C. for 5 hours. The mixture was cooled to room temperature, then basified to pH 10 using 10M aqueous sodium hydroxide, and extracted with dichloromethane. The combined extracts were washed with brine, dried and the solvent removed to leave a brown oil which was purified by vacuum distillation, b.p. 70° C. at 2 mbar.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05731335uspto-grants-1998_03