反应详情

温度

100 °C

A mixture of 4-bromo-2-fluorophenol (5 g, 30 mmol) and acetic anhydride (13.4 g, 130 mmol) in pyridine (10.6 ml, 130 mmol) was heated at 100° C. for 3 h and then brought to ambient temperature and poured into water. HCl (1 N and 6 N) was added and the solution was extracted with EtOAc. The combined organic phases were washed with sodium bicarbonate (saturated, 3×50 ml), dried (Na2SO4) and evaporated to dryness to give the title compound (5.8 g). MS m/z (rel. intensity, 70 eV) 233 (M+, 11), 232 (M+, 12), 191 (95), 190 (bp), 161 (8).

1. custombrought to ambient temperature
2. additionwas added
3. extractionthe solution was extracted with EtOAc
4. washThe combined organic phases were washed with sodium bicarbonate (saturated, 3×50 ml)
5. dry with materialdried (Na2SO4)
6. customevaporated to dryness