반응 #93736

ord-4bf628cb8a6b466a81e08fde37bc2f17

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과After the mixture was filtered
  2. 2
    농축the filtrate was concentrated in vacuo
  3. 3
    workup.ADDITIONthe concentrated liquid was poured into 50 ml of water
  4. 4
    추출The mixture was extracted with carbon tetrachloride
  5. 5
    세척After washing with water
  6. 6
    건조the resultant mixture was dried with anhydrous magnesium sulfate
  7. 7
    workup.DISTILLATIONthe solvent was then distilled off

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04614742uspto-grants-1986_09