反応 #93736

ord-4bf628cb8a6b466a81e08fde37bc2f17

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過After the mixture was filtered
  2. 2
    濃縮the filtrate was concentrated in vacuo
  3. 3
    workup.ADDITIONthe concentrated liquid was poured into 50 ml of water
  4. 4
    抽出The mixture was extracted with carbon tetrachloride
  5. 5
    洗浄After washing with water
  6. 6
    乾燥the resultant mixture was dried with anhydrous magnesium sulfate
  7. 7
    workup.DISTILLATIONthe solvent was then distilled off

実験手順

A 3.0 g amount of tetrafluoroisophthalonitrile and 1.26 g of 20 ml acetonitrile were dissolved in 20 ml of acetonitrile. A 1.66 g amount of sec-butanol was dropwise added to the mixture and the mixture was then stirred at room temperature for 24 hours. After the mixture was filtered, the filtrate was concentrated in vacuo and the concentrated liquid was poured into 50 ml of water. The mixture was extracted with carbon tetrachloride. After washing with water, the resultant mixture was dried with anhydrous magnesium sulfate and the solvent was then distilled off. Thus, 3.4 g (89% yield) of the desired compound No. 48 was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04614742uspto-grants-1986_09