HRID2352739

反应详情

EQUATION

反应方程式

HRID 2352739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

While stirring at room temperature, 4.8 g *28.5 mmol) of 2-phenyl-6-methyl-pyridine were dissolved in 50 ml of chloroform after which a solution of 7.8 g of 75% mCPBA (33.9 mmol) in 75 ml of chloroform were added dropwise. The reaction mixture showed only a slight rise in temperature. After stirring for 1.5 hr, the reaction mixture was shaken twice with 5% aqueous NaHCO3 solution and twice with an aqueous solution of Na2S2O3 to remove the excess of mCPBA, after which the reaction mixture proved to be negative on wet Kl/starch paper, The organic layer was dried on MgSO4. Removal of the drying agent by filtration and solvent by evaporation in vacuo yielded an oil which crystallized upon scratching to give 5.5 g (105%) of crude of 2-phenyl-6-methyl-pyridine-N-oxide, which was employed in the next step without further purification.

WORKUP

后处理

  1. additionwere added dropwise
  2. stirringAfter stirring for 1.5 hr
  3. customto remove the excess of mCPBA
  4. customThe organic layer was dried on MgSO4
  5. customRemoval of the drying agent
  6. filtrationby filtration and solvent
  7. customby evaporation in vacuo
  8. customyielded an oil which
  9. customcrystallized