反应详情

温度

0 °C

To 5-carboxy-1,3-benzodioxole (50 g, 300 mmol) in trifluoroacetic acid (400 mL) at 0° C. was added HNO3 (38 mL, 900 mmol) dropwise. The reaction mixture was stirred at 0° C. for 1 hour, then warmed to ambient temperature and stirred for 3 hours. The mixture was poured into ice water and the resulting precipitate was collected by filtration. The solid was air dried overnight to afford 58 g (92% yield) of 5-carboxy-6-nitro-1,3-benzodioxole as a yellow solid; NMR (DMSO-d6) 7.6 (s, 1), 7.3 (s, 1), 6.3 (s, 2) ppm.

1. temperaturewarmed to ambient temperature
2. stirringstirred for 3 hours
3. filtrationthe resulting precipitate was collected by filtration
4. customdried overnight