反应详情

To a suspension of 2.10 g (10.1 mmol) of 2-methoxy-5-tert-butylbenzoic acid in 6 mL of conc H2SO4 cooled in an ice bath was added dropwise a solution of 1 mL (11.1 mmol) of HNO3 in 2 ml H2SO4. The mixture was stirred, warming from 0° C. to rt over 3 h. The mixture was then poured into crushed ice and the resulting precipitate was filtered and dried. Recrystallization from 1:1 water/EtOH (8 mL/g) provided 1.4 g of product Intermediate 10.

1. temperaturecooled in an ice bath
2. temperaturewarming from 0° C. to rt over 3 h
3. additionThe mixture was then poured
4. custominto crushed ice
5. filtrationthe resulting precipitate was filtered
6. customdried
7. customRecrystallization from 1:1 water/EtOH (8 mL/g)