反应详情

To a stirred solution of 5-bromo-4-methylthiophene-2-sulfonamide (3.1 g, 12.1 mmol) in AcOH (30 mL) is added zinc dust (2.4 g, 36.2 mmol). The reaction mixture is heated to reflux for 8 hr. After 8 hr, the reaction mixture is cooled and filtered. The filtrate is neutralized with 1 M NaOH. The aqueous layer is extracted with EtOAc (300 mL). The organics are dried (Na2SO4), filtered and concentrated in vacuo. The crude product is chromatographed on silica gel, eluting with CH2Cl2 to afford the title compound (0.90 g, 43%).

1. temperatureThe reaction mixture is heated
2. temperatureto reflux for 8 hr
3. temperaturethe reaction mixture is cooled
4. filtrationfiltered
5. extractionThe aqueous layer is extracted with EtOAc (300 mL)
6. dry with materialThe organics are dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe crude product is chromatographed on silica gel
10. washeluting with CH2Cl2