反应详情

In a 100 mL round-bottomed flask was added sodium hydride (0.6 g) in tetrahydrofuran (10 ml) to give a suspension. 2-(2-Methoxyethoxy)ethanethiol (1 g) was added slowly. After the mixture stirred for 30 minutes, 4-fluoro-3-nitrobenzenesulfonamide (1.616 g) in 10 ml tetrahydrofuran was added slowly. After the mixture stirred overnight, water was added slowly, and ethyl acetate (20 ml×3) was used to extract the product. The combined organic layers were dried over Na2SO4. After the mixture was filtered and concentrated, the crude product was added to a silica gel column and purified eluting with 0-10% methanol in dichloromethane.

1. customto give a suspension
2. stirringAfter the mixture stirred overnight
3. extractionto extract the product
4. dry with materialThe combined organic layers were dried over Na2SO4
5. filtrationAfter the mixture was filtered
6. concentrationconcentrated
7. additionthe crude product was added to a silica gel column
8. custompurified
9. washeluting with 0-10% methanol in dichloromethane