HRID435494

反应详情

EQUATION

反应方程式

HRID 435494 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Phenol (3.0 g.) was converted into its sodium salt by dissolving in a freshly prepared sodium methoxide-methanol solution (0.7 g. of metallic sodium in 50 ml. of absolute methanol), and subsequent evaporation of the excess methanol under reduced pressure on a rotary evaporator. The solid residue was dissolved in acetonitrile (250 ml.) by stirring with 18-crown-6 (0.9 g.) for 30 minutes at room temperature. N-(1-methylethyl)-3-phenyl-2-oxiranecarboxamide (6.16 g.) was added to the solution, and the resulting mixture was heated under reflux for 6 hours. After cooling to room temperature, it was filtered. The filtrate was evaporated on a rotary evaporator under reduced pressure to give a resinous material. Water (ca. 200 ml.) was added to the residue, and allowed to stand at room temperature. The white precipitate thus separated was collected on a filter and washed with water. The filter residue was dried in air, then recrystallized from ethanol, giving 2.5 g. of product, m.p. 166°-168°.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 6 hours
  3. filtrationit was filtered
  4. customThe filtrate was evaporated on a rotary evaporator under reduced pressure
  5. customto give a resinous material
  6. customto stand at room temperature
  7. customThe white precipitate thus separated
  8. customwas collected on
  9. filtrationa filter
  10. washwashed with water
  11. customThe filter residue was dried in air
  12. customrecrystallized from ethanol
  13. customgiving 2.5 g