反应详情

温度

-3 °C

A mixture of N-(4-chloro-2-fluorophenyl)-1-cyclohexene-1,2-dicarboximide (24.4 g, 86.7 mmol) in sulfuric acid is cooled to −3° C., treated dropwise with 70% nitric acid (6.7 mL, 104.0 mmol) while maintaining the temperature from 0° to 2° C., warmed to and stirred at room temperature for 90 minutes, and poured onto ice. The resultant aqueous mixture is filtered to obtain a solid. The solid is washed with water and air-dried overnight to give the title product as a white powder (28.68 g, mp 152-155° C.) which is identified by 1H, 13C and 19F NMR spectral analyses.

1. temperaturewhile maintaining the temperature from 0° to 2° C.
2. temperaturewarmed to and
3. additionpoured onto ice
4. filtrationThe resultant aqueous mixture is filtered
5. customto obtain a solid
6. washThe solid is washed with water
7. customair-dried overnight