反应详情

温度

25 °C

To a solution of 10 g of salicylhydrazide in 100 ml of p-dioxane was added dropwise 13.1 g of trichloromethyl chloroformate while maintaining the temperature at 20°-30° C. with external cooling. After stirring at 25° C. for 0.5 hours, the suspension was refluxed for 4 hours then cooled to 25° C. and poured into excess ice-water. The mixture was filtered and the residue was recrystallized from acetonitrile to yield 9.0 g of the subject compound; m.p. 198°-200° C.

1. temperaturewhile maintaining the temperature at 20°-30° C. with external cooling
2. temperaturethe suspension was refluxed for 4 hours
3. temperaturethen cooled to 25° C.
4. filtrationThe mixture was filtered
5. customthe residue was recrystallized from acetonitrile