反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4,6-Dimethylpyrimidin-2-ol (10.0 g, 80.6 mmol) was added to sulfuric acid (80 mL) at 0° C. Then potassium nitrate (16.29 g, 161.1 mmol), was added to the reaction mixture at 0° C. The mixture was stirred at room temperature for 24 hr. The reaction mixture was poured slowly into diethyl ether (1000 mL) at 0° C. The precipitated solid was collected by filtration and washed with diethyl ether. A suspension of the solid in ethanol (50.0 mL) was neutralized with sodium hydrogen carbonate at room temperature. The solid was removed by filtration and the filter cake was washed with ethanol (ca. 3000 mL). The filtrate was concentrated in vacuo to give the title compound (13.15 g) as a pale yellow solid.
WORKUP
后处理
- filtrationThe precipitated solid was collected by filtration
- washwashed with diethyl ether
- additionA suspension of the solid in ethanol (50.0 mL)
- customwas neutralized with sodium hydrogen carbonate at room temperature
- customThe solid was removed by filtration
- washthe filter cake was washed with ethanol (ca. 3000 mL)
- concentrationThe filtrate was concentrated in vacuo