反应 #2439921

反应方程式

2-phenyl-6-methyl-pyridine

mCPBA

NaHCO3

Na2S2O3

→

2-phenyl-6-methyl-pyridine-N-oxide

溶剂

chloroform

chloroform

反应条件

后处理

1. 1
   workup.ADDITIONwere added dropwise
2. 2
   workup.STIRRINGAfter stirring for 1.5 hr
3. 3
   其他to remove the excess of mCPBA
4. 4
   其他The organic layer was dried on MgSO4
5. 5
   其他Removal of the drying agent
6. 6
   过滤by filtration and solvent
7. 7
   其他by evaporation in vacuo
8. 8
   其他yielded an oil which
9. 9
   其他crystallized

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.

来源