反应详情

温度

0 °C

A 0° C. solution of 3-methyl-2-(methylthio)pyrimidin-4(3H)-one (1.37 g, 8.77 mmol) in CHCl3 (15 mL) was treated with bromine (0.54 mL, 10.5 mmol), stirred at 0° C. for 1 h, quenched with satd. NaHCO3 (15 mL), warmed to RT slowly and stirred overnight. The mixture was extracted with DCM (3×) and the combined organics were dried over Na2SO4 and concentrated to dryness to afford 5-bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one (2.0 g, 97% yield). 1H NMR (400 MHz, DMSO-d6): δ 8.24 (s, 1H), 3.45 (s, 3H), 2.55 (s, 3H); MS (ESI) m/z: 235.0 (M+H+).

1. customquenched with satd
2. temperatureNaHCO3 (15 mL), warmed to RT slowly
3. stirringstirred overnight
4. extractionThe mixture was extracted with DCM (3×)
5. dry with materialthe combined organics were dried over Na2SO4
6. concentrationconcentrated to dryness