反応 #93728

反応方程式

tetrafluoroisophthalonitrile

acetonitrile

sodium bicarbonate

→

desired compound

収率 61.0%

4-Amino-2,5,6-trifluoroisophthalonitrile

収率 61.0%

溶媒

ammonia

反応条件

後処理

1. 1
   workup.ADDITIONAfter the dropwise addition
2. 2
   抽出the resultant mixture was extracted with chloroform
3. 3
   洗浄was washed with an aqueous sodium chloride solution
4. 4
   乾燥After drying with sodium sulfate
5. 5
   workup.DISTILLATIONthe chloroform was distilled off
6. 6
   その他to obtain yellow crystal
7. 7
   その他The resultant crystal was recrystallized from chloroform

実験手順

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.

出典