反应详情

温度

25 °C

The solution of bromine (5.1 g, 31.9 mmol) in chloroform (30 mL) was added dropwise to the solution of 2,6-dimethylpyrimidin-4-ol (3.43 g, 27.6 mmol) in chloroform (50 mL) at 0° C. Then the mixture was stirred at 25° C. for 12 hours. Saturated sodium sulfite solution was added to the mixture until the colour of the mixture changed to colourless. The organic phase was separated, dried over sodium sulphate, filtered, and then concentrated to give a residue. The residue was purified by column chromatography (silica gel, dichloromethane/methanol=15:1) to give 5-bromo-2,6-dimethylpyrimidin-4-ol as a white solid (3.7 g, 66%). 1H NMR (300 MHz, d6-DMSO): δ 2.33 (s, 3H), 2.24 (s, 3H).

1. customThe organic phase was separated
2. dry with materialdried over sodium sulphate
3. filtrationfiltered
4. concentrationconcentrated
5. customto give a residue
6. customThe residue was purified by column chromatography (silica gel, dichloromethane/methanol=15:1)