反应详情

温度

80 °C

3-trifluoromethyl-2-pyridinol (25 g, 153.3 mmol) is dissolved in anhydrous CH3CN (150 mL) and DMF (150 mL). N-iodosuccinimide (34.5 g, 153 mmol) is then added. The reaction mixture is stirred at 80° C. for 2 hours and cooled to room temperature. Aqueous 1 M NaHCO3 (150 mL) is then added to the cooled mixture. After stirring for 5 min, the solvents are evaporated to dryness. Water is added and the aqueous phase is extracted (×2) with dichloromethane. The organic phase is then evaporated and the desired product is recrystallized in water to afford 36.2 g (81%) of a white powder.

1. temperaturecooled to room temperature
2. stirringAfter stirring for 5 min
3. customthe solvents are evaporated to dryness
4. additionWater is added
5. extractionthe aqueous phase is extracted (×2) with dichloromethane
6. customThe organic phase is then evaporated
7. customthe desired product is recrystallized in water