反应详情

To 6.8 g (0.04 mole) 2-hydroxybenzenesulfonamide in 100 ml methylene chloride was added 4.4 g (0.044 mole) triethylamine and 6.3 g (0.044 mole) dimethylsulfamoyl chloride in 5 ml methylene chloride, keeping the reaction temperature <10° C. The mixture was then warmed to room temperature and stirred 72 hours. The reaction mixture was then diluted with 100 ml methylene chloride washed with 100 ml water, 100 ml 1% HCl and dried over MgSO4. The solvent was evaporated to give a crude yellow oil that slowly solidified on standing. The solids were then triturated with hexanes and filtered to give 6.1 g of a tan solid, m.p. 88°-89° C.

1. customthe reaction temperature <10° C
2. washwashed with 100 ml water, 100 ml 1% HCl
3. dry with materialdried over MgSO4
4. customThe solvent was evaporated
5. customto give a crude yellow oil that
6. customThe solids were then triturated with hexanes
7. filtrationfiltered