反应详情

To a solution of 10 (19.0 g, 139.6 mmol) in acetic acid (180 mL) was added a solution of fuming HNO3 (10 mL) in acetic acid (70 mL) dropwise over 30 minutes. The mixture was stirred at ambient temperature for 10 minutes, then poured into a beaker containing ice to give a crystalline precipitate, which was collected by vacuum filtration and washed with water to afford the crude product. Further purification via recrystallization from CH2Cl2/hexane gave the pure product (16.3 g, 64.4%).

1. additionpoured into a beaker
2. additioncontaining ice
3. customto give a crystalline precipitate, which
4. filtrationwas collected by vacuum filtration
5. washwashed with water
6. customto afford the crude product
7. customFurther purification
8. customvia recrystallization from CH2Cl2/hexane