반응 #93728

ord-a6445229094340d9a835bd8167833b6b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the dropwise addition
  2. 2
    추출the resultant mixture was extracted with chloroform
  3. 3
    세척was washed with an aqueous sodium chloride solution
  4. 4
    건조After drying with sodium sulfate
  5. 5
    workup.DISTILLATIONthe chloroform was distilled off
  6. 6
    기타to obtain yellow crystal
  7. 7
    기타The resultant crystal was recrystallized from chloroform

실험 절차

To a solution of 2.0 g of tetrafluoroisophthalonitrile in 20 ml of acetonitrile, 0.6 ml of 28% aqueous ammonia was dropwise added. After the dropwise addition, the mixture was stirred at room temperature for one hour. An aqueous sodium bicarbonate solution was added to the mixture and the resultant mixture was extracted with chloroform and was washed with an aqueous sodium chloride solution. After drying with sodium sulfate, the chloroform was distilled off to obtain yellow crystal. The resultant crystal was recrystallized from chloroform to obtain 1.2 g (61% yield) of the desired compound No. 1.

출처

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