反应详情

温度

55 °C

To a solution of fuming nitric acid (18 mL) and glacial acetic acid (36 mL) preheated to 55° C. was added 3-fluoro-5-methoxybenzoic acid (3.00 g, 17.63 mmol) portion wise over 5 min. The mixture was maintained at 55° C. for an additional 90 min. The reaction was cooled to ambient temperature and poured onto ice-water (200 mL). The pH of the solution was adjusted to 2 using aqueous NaHCO3 solution. The precipitate formed was filtered and washed with hexanes (100 mL) to afford 5-fluoro-3-methoxy-2-nitrobenzoic acid (2.52 g, 66%) as a white solid. 1H NMR and MS consistent.

1. custompreheated to 55° C.
2. temperatureThe reaction was cooled to ambient temperature
3. additionpoured onto ice-water (200 mL)
4. customThe precipitate formed
5. filtrationwas filtered
6. washwashed with hexanes (100 mL)