반응 #93737

반응 방정식

tetrafluoroisophthalonitrile

potassium fluoride

water

n-butylmercaptan

→

desired compound

수율 77.0%

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

수율 77.0%

용매

acetonitrile

반응 조건

후처리

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

실험 절차

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.

출처