反应详情

温度

50 °C

23.6 g of zinc powder are added to a suspension of 22.0 g of N-tert.-butyl-2-dimethylaminocarbonyl-5-nitro-benzenesulfonamide (Example d), 18.2 g of ammonium chloride, 70 ml of water and 150 ml of methanol. The mixture is then stirred at 50° C. When the reaction has ended, the solid is filtered off. After the solid has been washed with ethyl acetate, the filtrate is concentrated, the residue is taken up in ethyl acetate and the mixture is washed with water. After drying over MgSO4, the organic phase is concentrated and the residue is washed with diisopropyl ether; yield: 17.5 g; m.p.: 205-208° C.

1. filtrationthe solid is filtered off
2. washAfter the solid has been washed with ethyl acetate
3. concentrationthe filtrate is concentrated
4. washthe mixture is washed with water
5. dry with materialAfter drying over MgSO4
6. concentrationthe organic phase is concentrated
7. washthe residue is washed with diisopropyl ether