HRID657660

反应详情

EQUATION

反应方程式

HRID 657660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 4-(4-methoxyphenyl)-2-methylpyridine 1-oxide (384 mg) in a 48% aqueous solution of hydrobromic acid (2.08 mL) is heated under reflux for 4 hours. The mixture is allowed to cool back to room temperature, water and ethyl acetate are added and the two phases separated by decantation. The aqueous phase is concentrated under reduced pressure. The residue is dissolved in chloroform (4 mL); triethylamine (1 equivalent) is added followed by metachloroperbenzoic acid (1 equivalent). The mixture is stirred for two hours at room temperature; a few drops of methanol are added to dissolve the reactants and stirred again for one hour at room temperature. Concentration under reduced pressure affords 55 mg of 4-(4-hydroxyphenyl)-2-methylpyridine 1-oxide as a yellow oil used without further purification.

WORKUP

后处理

  1. temperatureunder reflux for 4 hours
  2. customthe two phases separated by decantation
  3. concentrationThe aqueous phase is concentrated under reduced pressure
  4. dissolutionThe residue is dissolved in chloroform (4 mL)
  5. dissolutionto dissolve the reactants
  6. stirringstirred again for one hour at room temperature
  7. concentrationConcentration under reduced pressure