反应详情

A 1.1 g (0.012 mol) sample of methylsulfenyl chloride was added dropwise to a cooled (-5° to -10° C.) solution of 3.6 g (0.01 mol) 4-dipropylamino-N-methyl-3,5-dinitrobenzenesulfonamide and 1.1 g (0.014 mol) pyridine in 25 ml dichloromethane. The reaction mixture was then stirred at about 0° C. until the sulfonamide reactant could not be detected by thin layer chromatography on silica gel (benzene/acetone eluant). The reaction mixture was then washed with water, dried over magnesium sulfate and evaporated under reduced pressure to give a yellow semi-solid residue. The residue was recrystallized from ethanol to give 2.3 g of the product, as a yellow solid, m.p. 119°-121° C. Elemental analysis for C14H22N4O6S2 showed: % S, calc. 15.8, found 15.9.

1. washThe reaction mixture was then washed with water
2. dry with materialdried over magnesium sulfate
3. customevaporated under reduced pressure
4. customto give a yellow semi-solid residue
5. customThe residue was recrystallized from ethanol