反応 #93729

反応方程式

sodium bicarbonate

tetrafluoroisophthalonitrile

triethylamine

aniline

→

desired compound

収率 91.6%

4-Anilino-2,4,6-trifluoroisophthalonitrile

収率 91.6%

溶媒

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONAfter dropwise adding
2. 2
   抽出The mixture was extracted with chloroform
3. 3
   抽出the chloroform extract
4. 4
   洗浄was washed 5 times with an aqueous sodium chloride solution
5. 5
   乾燥After drying with magnesium sulfate
6. 6
   workup.DISTILLATIONthe chloroform was distilled off
7. 7
   その他The resultant crude crystal was purified by silica gel chromatography (solvent:hexane)

実験手順

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.

出典