反応 #936154

ord-7847eeef3ca3484da4f61f58a372e803

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was refluxed for 6 hours
  2. 2
    温度cooled
  3. 3
    抽出followed by extraction with ethyl acetate (4×100 ml)
  4. 4
    乾燥dried (MgSO4)
  5. 5
    その他the solvent removed

実験手順

The crude 6-ethoxy-5,6-dihydro-2-[3-(trifluoromethyl)phenyl]-4H-1,3,4-oxadiazine-4-carboxylic acid ethyl ester (17 g) from Step C above, was mixed with 12 g of KOH, 20 g of ethanol, and 40 g of water to create a reaction mixture. The reaction mixture was refluxed for 6 hours and then cooled. 50 ml of water was then added to the reaction mixture, followed by extraction with ethyl acetate (4×100 ml). The ethyl acetate extracts were conbined, dried (MgSO4) and the solvent removed, to give 7 g of crude 6-ethoxy-5,6-dihydro-2-[3-(trifluoromethyl)phenyl]-4H-1,3,4-oxadiazine, which was not purified and was used in Step E below.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06011034uspto-grants-2000_01