反应详情

A solution of 50 g (0.305 mole) 3,4-methylenedioxy-acetophenone (Aldrich) in 200 mL glacial acetic acid was added dropwise over 30 minutes to 700 mL of cold (2–4° C.) 70% HNO3 with stirring (NOTE: the reaction will overheat without external cooling from an ice bath, which can be dangerous and lead to side products). At temperatures below 0° C., however, the reaction can be sluggish. A temperature of 3–5° C. seems to be optimal). The mixture was left stirring for another 60 minutes at 3–5° C., and then allowed to approach ambient temperature. Analysis by TLC (25% EtOAc in hexane) indicated complete conversion of the starting material within 1–2 hr. When the reaction was complete, the mixture was poured into ˜3 liters of crushed ice, and the resulting yellow solid was filtered off, washed with water and then suction-dried. Yield 53 g (84%), used without further purification.

1. customthe reaction
2. temperaturewithout external cooling from an ice bath
3. customAt temperatures below 0° C., however, the reaction
4. customA temperature of 3–5° C.
5. waitThe mixture was left
6. stirringstirring for another 60 minutes at 3–5° C.
7. customto approach ambient temperature
8. customwithin 1–2 hr
9. filtrationthe resulting yellow solid was filtered off
10. washwashed with water
11. customsuction-dried
12. customYield 53 g (84%), used without further purification