116529-61-4

400629-31-4

116529-61-4

General procedure for the synthesis of 3-bromo-2-nitrobenzoic acid from 2-(3-bromo-2-nitrophenyl)acetic acid: to a 500 mL three-necked flask was added 500 mL of water and 10.0 g of sodium hydroxide, followed by 24.0 g of 2-(3-bromo-2-nitrophenyl)acetic acid. The reaction mixture was heated to 90 °C and kept at this temperature for 6 hours. After completion of the reaction, it was cooled to room temperature, filtered to remove insoluble material and the filtrate was collected. The pH of the filtrate was adjusted to 1.5 with concentrated hydrochloric acid and extracted with ethyl acetate (80 mL each time, 3 times). The organic phases were combined, washed with saturated brine and dried with anhydrous sodium sulfate. The organic phase was concentrated under reduced pressure to give 19.1 g (84.1% yield) of 3-bromo-2-nitrobenzoic acid.