反应详情

温度

-30 °C

N-formylmorpholine (3 ml) and 2.05 g of anhydrous sodium saccharin were added to 10 ml of dichloromethane. The mixture was cooled to -30° C., and with stirring, 1.65 ml (corresponding to about 5 millimoles of phosgene) of a carbon tetrachloride solution containing 30% of phosgene (W/V %) was added. The temperature of the mixture was raised to room temperature over a period of about 1 hour and stirred at room temperature for 2 hours. The solvent was distilled off under reduced pressure. Water was added to the remaining oily product, and under ice cooling, the mixture was stirred until the oily product crystallized. The crystals were collected by filtration, thoroughly washed with water, and dried to afford 1.70 g of white crystals (yield 73.4%), decomposition point:160°-169° C. Recrystallization of the crude crystals from acetone yielded white needle-like crystals having a decomposition point of 173° to 175° C.

1. additionwas added
2. temperatureThe temperature of the mixture was raised to room temperature over a period of about 1 hour
3. stirringstirred at room temperature for 2 hours
4. distillationThe solvent was distilled off under reduced pressure
5. additionWater was added to the remaining oily product
6. stirringunder ice cooling, the mixture was stirred until the oily product
7. customcrystallized
8. filtrationThe crystals were collected by filtration
9. washthoroughly washed with water
10. customdried