反应详情

温度

80 °C

9.0 g (76 millimoles) of 4-chlorobutan-2-one were slowly added dropwise to 10.0 g (50 millimoles) of sodium saccharin in 100 ml of absolute dimethylformamide, while stirring. The temperature was then gradually increased to 80° C., and the reaction mixture was stirred at this temperature for 5 hours, after which it was cooled. An excess of ice-water was added, and stirring was continued for a further hour. The precipitated solid was filtered off under suction, recrystallized from ethanol and dried in a drying oven under reduced pressure at 50° C. to give 10.9 g (86%) of N-(2-oxobut-4-yl)-saccharin of melting point 118°-119° C.

1. stirringthe reaction mixture was stirred at this temperature for 5 hours
2. temperatureafter which it was cooled
3. stirringstirring
4. waitwas continued for a further hour
5. filtrationThe precipitated solid was filtered off under suction
6. customrecrystallized from ethanol
7. customdried in a drying oven under reduced pressure at 50° C.