反応 #2267070

ord-a9a61f4ca8f04b30a8369b6436cc3cd4

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The resulting solution was heated
  2. 2
    温度to reflux for 3 hours
  3. 3
    その他The solvent was removed under reduced pressure
  4. 4
    workup.ADDITIONThe residue was treated with NaHCO3
  5. 5
    抽出extracted with ethyl acetate
  6. 6
    洗浄The combined organic phase was washed with brine
  7. 7
    乾燥dried over Na2SO4
  8. 8
    その他Removal of the solvent

実験手順

To a solution of 4 (1.6 g) in 25 ml of ethanol was added acetic hydrazide (0.4 g) and 2 drops of concentrated HCl. The resulting solution was heated to reflux for 3 hours. The solvent was removed under reduced pressure. The residue was treated with NaHCO3, and extracted with ethyl acetate. The combined organic phase was washed with brine, dried over Na2SO4. Removal of the solvent gave the desired product (1.25 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06887867B2uspto-grants-2005_05