HRID420682

反应详情

EQUATION

反应方程式

HRID 420682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(2,2-Dimethyl-1,3-dioxan-5-yl)-6-(methyloxy)pyrido[2,3-b]pyrazin-3(4H)-one (17.40 g, 59.7 mmol) was dissolved in THF (220 ml) to give a dark yellow solution. 1M HCl aq. (200 ml) was added (transient blue and green colours appeared in the solution) and the now light yellow solution was stirred at room temperature for 1 h. The mixture was concentrated to ca. 300 ml on a rotary evaporator using a cold water bath (some solid was precipitated during this procedure) then was stirred vigorously while solid sodium hydrogen carbonate was added in portions (caution: effervescence) until the mixture was ca. pH 8. The resulting yellow solid was collected by filtration with suction, washed with water (2×20 ml) and air-dried to give the title compound as an amorphous yellow solid (13.805 g, 91%).

WORKUP

后处理

  1. customto give a dark yellow solution
  2. concentrationThe mixture was concentrated to ca. 300 ml on a rotary evaporator
  3. customwas precipitated during this procedure)
  4. stirringthen was stirred vigorously while solid sodium hydrogen carbonate
  5. additionwas added in portions (caution: effervescence) until the mixture
  6. filtrationThe resulting yellow solid was collected by filtration with suction
  7. washwashed with water (2×20 ml)
  8. customair-dried