反应详情

温度

60 °C

5-Chlorosalicylic acid (20 g, 115.8 mmol) is dissolved in DMF (100 mL). To this solution is added NIS (26.1 g, 116.0 mmol) which causes the reaction to warm up to 60° C. The reaction is stirred at room temperature for 20 hours. At this point ethyl acetate (100 mL) is added and the solution washed with 0.1N HCl (100 mL). The organic phase is then washed with water (3×100 mL), dried with sodium sulfate and evaporated under reduced pressure to yield 5-yield 5-chloro-3-iodosalicylic acid as off-white solid. (mp 160°-163° C.)

1. customthe reaction
2. washthe solution washed with 0.1N HCl (100 mL)
3. washThe organic phase is then washed with water (3×100 mL)
4. dry with materialdried with sodium sulfate
5. customevaporated under reduced pressure