HRID255819

反应详情

EQUATION

反应方程式

HRID 255819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

To a solution containing 0.62 g of potassium hydroxide in 50 ml of methanol was added 3 g of the oxadiazole prepared in Example 2. After stirring about five minutes, 2 g of methyl iodide was added. The suspension was refluxed 0.5 hour, cooled to 30° C., an extra 10 g of methyl iodide was added, and the suspension was refluxed an additional two hours, then concentrated in vacuo. After water was added to the residue, the suspension was filtered and the solid was washed with 1×50 ml of water. The suction-dried solid was recrystallized from 2-propanol to give 2 g of the subject compound: m.p. 138°-140° C.

WORKUP

后处理

  1. temperatureThe suspension was refluxed 0.5 hour
  2. temperaturethe suspension was refluxed an additional two hours
  3. concentrationconcentrated in vacuo
  4. additionAfter water was added to the residue
  5. filtrationthe suspension was filtered
  6. washthe solid was washed with 1×50 ml of water
  7. customThe suction-dried solid was recrystallized from 2-propanol