反应详情

4-Methylthiobenzonitrile (12 g) was dissolved in a 4N solution of hydrogen chloride in ethyl acetate (130 mL). To this solution was added O,O-diethyl dithiophosphate (15 mL) and the mixture was stirred at room temperature for 22 hours. Water (100 mL) was added to the reaction mixture and extracted with ethyl acetate. After the insoluble materials were filtered off, the filtrate was washed with a saturated aqueous solution of sodium chloride and dried and, thereafter, the solvent was distilled off. The residue was recrystallized from ethyl acetate to obtain 10 g of the title compound (yield 67%).

1. extractionextracted with ethyl acetate
2. filtrationAfter the insoluble materials were filtered off
3. washthe filtrate was washed with a saturated aqueous solution of sodium chloride
4. customdried
5. distillationthe solvent was distilled off
6. customThe residue was recrystallized from ethyl acetate