反应详情

A mixed acid was prepared by adding fuming nitric acid (1 mL), which was added 3 times as divided portions, to concentrated sulfuric acid (6 mL) under ice cooling, and added portionwise with 4-acetamidobenzaldehyde (1.91 g, 11.7 mmol). After the addition, the reaction mixture was immediately poured onto ice, and the solids were collected by filtration. The solids were sufficiently washed with cold water, dried, purified by silica gel column chromatography (developing solvent: CH2Cl2), and then recrystallized from water to obtain the target compound as pale yellow needlelike solid (1.57 g, yield: 64%).

1. customA mixed acid was prepared
2. additionwas added 3 times
3. additionAfter the addition
4. additionthe reaction mixture was immediately poured onto ice
5. filtrationthe solids were collected by filtration
6. washThe solids were sufficiently washed with cold water
7. customdried
8. custompurified by silica gel column chromatography (developing solvent: CH2Cl2)
9. customrecrystallized from water