反应详情

温度

0 °C

To a solution of 1,6-dimethylpyrimidine-2,4(1H,3H)-dione (5 g, 0.035 mol) in H2SO4 (20 mL) at 0° C. was added dropwise a solution of KNO3 (4.69 g, 0.046 mol) in H2SO4 (10 mL). The reaction was stirred 0° C. for 2 h, warmed to RT, stirred for 18 h, poured into ice then extracted with EA (5×50 mL). The combined organic layers were dried over Na2SO4, and concentrated to give 1,6-dimethyl-5-nitropyrimidine-2,4(1H,3H)-dione (4.3 g, 68.1% yield) as a yellow solid. 1H NMR (DMSO-d6) δ: 12.09 (s, 1H), 3.32 (s, 3H), 2.36 (s, 3H) LCMS: MH+ 186 and TR=0.610 min. Used without further purification.

1. temperaturewarmed to RT
2. stirringstirred for 18 h
3. additionpoured into ice
4. extractionthen extracted with EA (5×50 mL)
5. dry with materialThe combined organic layers were dried over Na2SO4
6. concentrationconcentrated