反应详情

温度

35 °C

4-Nitrobenzenesulphonamide (2.02 g, 10 mmol) was added to a solution of 1,3,5-trioxane (1.96 g, 20 mmol) in acetic acid (5 ml). The mixture was cooled for 5 minutes ated methanesulphonic acid (10 ml) was added slowly. The mixture was then stirred at 35° C. for 20 minutes, cooled to 0° C., diluted with water and extracted with ethyl acetate. The combined extracts were washed twice with water and twice with 5% aqueous sodium hydrogen carbonate solution, then dried and the volatiles removed by evaporation. The residue was recrystallized from ethanol to give the title compound (955 mg, 35%). NMR: 4.87 (s, 2H), 5.30 (s, 4H), 8.20 (d, 2H), 8.42 (d, 2H).

1. temperatureThe mixture was cooled for 5 minutes
2. additionwas added slowly
3. temperaturecooled to 0° C.
4. extractionextracted with ethyl acetate
5. washThe combined extracts were washed twice with water and twice with 5% aqueous sodium hydrogen carbonate solution
6. customdried
7. customthe volatiles removed by evaporation
8. customThe residue was recrystallized from ethanol