反应详情

To 2.13 g (10 mmole) of N-(4-acetylphenyl)methanesulfonamide in 50 ml of alcohol and 50 ml of water at 30° C. is added 1.43 g (10 mmol) of calcium hypochlorite. The solution is stirred for 24 hrs and an additional 1.43 g of calcium hypochlorite added. The mixture is stirred for 3 days at room temperature. The mixture is acidified with acetic acid to pH 6; concentrated and extracted into water-methylene chloride. The organic layer is dried, evaporated and the residue flash chromatographed on silica gel eluting in succession with 25% and 50% ethyl acetate-pet. ether. The solid product is recrystallized from Et2O-pet. ether; m.p. 129°-131° C. MW 247.71.

1. stirringThe mixture is stirred for 3 days at room temperature
2. concentrationconcentrated
3. extractionextracted into water-methylene chloride
4. customThe organic layer is dried
5. customevaporated
6. customthe residue flash chromatographed on silica gel eluting in succession with 25% and 50% ethyl acetate-pet. ether
7. customThe solid product is recrystallized from Et2O-pet. ether