反应详情

To a stirred solution of 2-(imidazo[1,2-b][1,2,4]triazin-3-yl)propan-2-ol (5.55 g, 31.1 mmol) in acetic acid (100 ml) was added sodium acetate (3.83 g, 46.7 mmol), then, dropwise over 5 min, a solution of bromine (1.77 ml, 34.4 mmol) in acetic acid (12 ml). The solution was stirred at room temperature for 25 min, then partitioned between saturated aqueous NaHCO3 (2 l) and ethyl acetate (1 l). The aqueous layer (pH 7) was further extracted with ethyl acetate (1 l), and the combined organic extracts were dried (Na2SO4) and evaporated iii, vacuo. The residue was purified by flash chromatography (silica gel, 2% MeOH/CH2Cl2) to afford 6.17 g (77%) of the title compound as a yellow solid: 1H NMR (360 MHz, CDCl3) δ 1.70 (6H, s), 3.12 (1H, br s), 7.95 (1H, s), 8.80 (1H, s).

1. custompartitioned between saturated aqueous NaHCO3 (2 l) and ethyl acetate (1 l)
2. extractionThe aqueous layer (pH 7) was further extracted with ethyl acetate (1 l)
3. dry with materialthe combined organic extracts were dried (Na2SO4)
4. customevaporated iii, vacuo
5. customThe residue was purified by flash chromatography (silica gel, 2% MeOH/CH2Cl2)