反应详情

温度

100 °C

A mixture of 4-bromo-2-hydroxy-benzoic acid (12.35 g, 56.91 mmol), acetic anhydride (35.6 mL) and conc sulfuric acid (0.93 mL) was heated at 100° C. for 1 h; then cooled, poured into 400 g ice/water, stirred for several minutes, the white precipitates were collected with filtration, washed with water, then the white solids were oven vacuum dried at 50° C. for 3 days to give the desired product (11.62 g). 1H NMR (200 MHz, CDCl3): δ (ppm)=7.95 (d, 1H, J=8.5 Hz), 7.48 (dd, 1H, J=2.0 Hz, 8.5 Hz), 7.32 (d, 1H, J=2.0 Hz).

1. temperaturethen cooled
2. customthe white precipitates
3. filtrationwere collected with filtration
4. washwashed with water
5. customdried at 50° C. for 3 days