Реакция #93729

ord-cc6b7dbb434043b799a779764f134485

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONAfter dropwise adding
  2. 2
    ЭкстракцияThe mixture was extracted with chloroform
  3. 3
    Экстракцияthe chloroform extract
  4. 4
    Промывкаwas washed 5 times with an aqueous sodium chloride solution
  5. 5
    СушкаAfter drying with magnesium sulfate
  6. 6
    workup.DISTILLATIONthe chloroform was distilled off
  7. 7
    ДругоеThe resultant crude crystal was purified by silica gel chromatography (solvent:hexane)

Методика

A solution of 0.85 g of aniline in 20 ml of acetonitrile was dropwise added, while stirring, to a solution of 2.0 g of tetrafluoroisophthalonitrile and 2.0 g of triethylamine in 30 ml of acetonitrile. After dropwise adding, the mixture was stirred at room temperature for 1 hour and an aqueous sodium bicarbonate solution was then added. The mixture was extracted with chloroform and the chloroform extract was washed 5 times with an aqueous sodium chloride solution. After drying with magnesium sulfate, the chloroform was distilled off. The resultant crude crystal was purified by silica gel chromatography (solvent:hexane). Thus, 2.3 g (87% yield) of the desired compound No. 6 was obtained.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04614742uspto-grants-1986_09