反应详情

温度

110 °C

In a 25 mL microwave tube was added sodium hydride (0.6 g) in terahydrofuran (10 mL) to give a suspension. 2-(2-Methoxyethoxy)ethanethiol (1 g) was added slowly. After stirring for 30 minutes, 3-chloro-4-fluorobenzenesulfonamide (1.54 g) dissolved in 10 mL tetrahydrofuran was added slowly. The mixture was heated at 110° C. for 30 minutes in a Biotage Initiator microwave reactor. Water was added, the product was extracted with ether (20 mL×3), dried over Na2SO4, filtered, and the solvent was removed under reduced pressure. The crude product was purified by flash chromatography on silica eluting with 0-25% ethyl acetate in hexane.

1. customto give a suspension
2. additionwas added slowly
3. extractionthe product was extracted with ether (20 mL×3)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customthe solvent was removed under reduced pressure
7. customThe crude product was purified by flash chromatography on silica eluting with 0-25% ethyl acetate in hexane