反応 #2439921

反応方程式

2-phenyl-6-methyl-pyridine

mCPBA

NaHCO3

Na2S2O3

→

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

溶媒

chloroform

chloroform

反応条件

後処理

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

実験手順

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.

出典