HRID1398951

反应详情

EQUATION

反应方程式

HRID 1398951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationThe precipitated solid was collected by filtration
  2. washwashed with diethyl ether
  3. additionA suspension of the solid in ethanol (50.0 mL)
  4. customwas neutralized with sodium hydrogen carbonate at room temperature
  5. customThe solid was removed by filtration
  6. washthe filter cake was washed with ethanol (ca. 3000 mL)
  7. concentrationThe filtrate was concentrated in vacuo