HRID65700

反应详情

EQUATION

反应方程式

HRID 65700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.7 g. of 8-ethyl-2-methyl-4H-pyrazolo[1,5-a]pyrazolo-[4',3':5,6]pyrido[3,4-e]pyrimidin-5(8H)-one (0.01 mol.) are added to a suspension of 0.03 g. of sodium hydride in 50 ml. of diethylene glycol dimethyl ether at reflux temperature. The temperature is maintained for one hour and then lowered to 120°. 2.8 g. of methyl iodide are added and heating is continued for 10 hours. The precipitated sodium iodide is filtered off, the solution evaporated to dryness and the residue recrystallized from ethyl-acetate, yield 1.9 g. (68%); m.p. 206°-207°.

WORKUP

后处理

  1. temperatureThe temperature is maintained for one hour
  2. customlowered to 120°
  3. temperatureheating
  4. filtrationThe precipitated sodium iodide is filtered off
  5. customthe solution evaporated to dryness
  6. customthe residue recrystallized from ethyl-acetate, yield 1.9 g