反应详情

After the addition of a spatula tip of 4-dimethylaminopyridine to a suspension of 4 g of the sodium salt of saccharin in 60 ml of methylene chloride, a solution of 3.9 g of benzo-1,2,3-thiadiazole-7-carboxylic acidchloride in 20 ml of methylene chloride is added dropwise at a maximum of 20° C. The mixture is stirred overnight at room temperature and thenext day the suspension is poured onto ice-water and extracted with ethyl acetate. The extracts are washed with dilute sodium hydrogen carbonate solution and water, dried and concentrated by evaporation. The residue is recrystallised from tetrahydrofuran/hexane to yield the title compound having a melting point of 173°-175° C.

1. additionis poured onto ice-water
2. extractionextracted with ethyl acetate
3. washThe extracts are washed with dilute sodium hydrogen carbonate solution and water
4. customdried
5. concentrationconcentrated by evaporation
6. customThe residue is recrystallised from tetrahydrofuran/hexane