反応 #93737

反応方程式

tetrafluoroisophthalonitrile

potassium fluoride

water

n-butylmercaptan

→

desired compound

収率 77.0%

2,4,5-Trifluoro-6-n-butylthioisophthalonitrile

収率 77.0%

溶媒

acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONwas gradually dropwise added to the mixture
2. 2
   抽出the reaction mixture was extracted with chloroform
3. 3
   洗浄the extract was then washed with a saturated aqueous sodium bicarbonate solution
4. 4
   乾燥by drying with anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONAfter distilling off the chloroform
6. 6
   workup.DISTILLATIONthe resultant crude product was distilled in vacuo

実験手順

A 2.0 g amount of tetrafluoroisophthalonitrile and 0.87 g of potassium fluoride were dissolved in 10 ml of acetonitrile. After cooling to a temperature of 0° C., 0.90 g (1.04 ml) of n-butylmercaptan was gradually dropwise added to the mixture and the resultant mixture was stirred at a temperature of 0° C. or less for 12 hours. After 50 ml of water was added to the reaction mixture, the reaction mixture was extracted with chloroform and the extract was then washed with a saturated aqueous sodium bicarbonate solution, followed by drying with anhydrous magnesium sulfate. After distilling off the chloroform, the resultant crude product was distilled in vacuo. Thus, 2.08 g (77% yield) of the desired compound No. 52 was obtained.

出典