反应详情

To a mixture of 30.1 g of N-acetyl-2,6-xylidine (0.18 mole) and 40 ml of acetic acid (0.70 mole) was added gradually 80 ml of concentrated sulfuric acid (0.50 mole) with stirring under ice-cooling. Then, to the mixture was added slowly 10 ml of fuming nitric acid (0.24 mole) in a manner such that the temperature of the reaction mixture did not exceed 10° C. The reaction mixture was returned to room temperature and, after stirring for 2 hours, poured onto ice. The resulting crystalline precipitate was collected by filtration and recrystallized from ethanol to give 35.5 g (92%) of the title compound (m.p. 171°-173° C.; pale yellow needles).

1. temperaturecooling
2. customdid not exceed 10° C
3. customwas returned to room temperature
4. stirringafter stirring for 2 hours
5. additionpoured onto ice
6. filtrationThe resulting crystalline precipitate was collected by filtration
7. customrecrystallized from ethanol