反应详情

温度

0 °C

3-Methyl-2-methylthio-3H-pyrimidin-4-one (Step 2, 3.31 g, 21.2 mmol) was dissolved in CHCl3 (50 mL) and cooled to 0° C. under Ar. Br2 (1.25 mL, 25.4 mmol) was added via syringe, and the reaction was stirred at 0° C. for 35 min, at which time TLC analysis indicated complete consumption of starting material. The reaction was quenched with 40 mL saturated NaHCO3, warmed to RT, and stirred overnight. The reaction was extracted with CH2Cl2 (3×25 mL), and the organic extracts were combined, dried over Na2SO4, filtered, and concentrated to give the title compound, which did not require further purification. MS (ESI pos. ion) m/z: 236. Calc'd for C6H7BrN2OS: 233.95.

1. customconsumption of starting material
2. customThe reaction was quenched with 40 mL saturated NaHCO3
3. temperaturewarmed to RT
4. stirringstirred overnight
5. extractionThe reaction was extracted with CH2Cl2 (3×25 mL)
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated