반응 #93729

반응 방정식

sodium bicarbonate

tetrafluoroisophthalonitrile

triethylamine

aniline

→

desired compound

수율 91.6%

4-Anilino-2,4,6-trifluoroisophthalonitrile

수율 91.6%

용매

acetonitrile

acetonitrile

반응 조건

후처리

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

실험 절차

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.

출처