反应详情

To a solution of 7-trifluoromethylimidazo[1,2-c]pyrimidine (1.9239 g, 10.3 mmol) in acetic acid (40 ml) was added sodium acetate (1.265 g, 15.4 mmol), then a solution of bromine (0.529 ml, 10.3 mmol) in acetic acid (7.5 ml). The solution was stirred at room temperature for 30 min, then partitioned between saturated aqueous NaHCO3 (1 l) and ethyl acetate (500 ml). The aqueous layer (pH 8) was further extracted with ethyl acetate (500 ml), and the combined organic extracts were dried (Na2SO4) and evaporated in vacuo. The residue was purified by flash chromatography (silica gel, 20% EtOAc/isohexane) to afford 0.88 g (34% over 2 steps) of the title compound as a white solid: 1H NMR (360 MHz, CDCl3) δ 7.81 (1H, s), 7.93 (1H, s), 9.09 (1H, s).

1. custompartitioned between saturated aqueous NaHCO3 (1 l) and ethyl acetate (500 ml)
2. extractionThe aqueous layer (pH 8) was further extracted with ethyl acetate (500 ml)
3. dry with materialthe combined organic extracts were dried (Na2SO4)
4. customevaporated in vacuo
5. customThe residue was purified by flash chromatography (silica gel, 20% EtOAc/isohexane)