Reacción #439972

Ecuación de reacción

Metachloroperbenzoic acid

2,3-dimethylpyridine

sodium sulfite

→

title compound

Rendimiento 50.1%

2,3-Dimethylpyridine N-oxide

Rendimiento 50.1%

Disolventes

methylene chloride

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturaby heating to room temperature
2. 2
   Otrothe resulting mixture was separated
3. 3
   SecadoThe organic layer was dried over anhydrous magnesium sulfate
4. 4
   Concentraciónthe filtrate was concentrated
5. 5
   Otrothe concentrate was purified by chromatography on a silica gel column (5% methanol—methylene chloride)
6. 6
   workup.ADDITIONPetroleum ether was added to the residue
7. 7
   OtroColorless powder so precipitated
8. 8
   Filtraciónwas collected by filtration
9. 9
   Otroby drying

Procedimiento

In methylene chloride (200 ml) was dissolved 2,3-dimethylpyridine (9.50 g) and the resulting solution was. cooled to 0° C. Metachloroperbenzoic acid (21.9 g) was added to the reaction mixture, followed by heating to room temperature. Stirring was conducted for 3 days. An aqueous solution of sodium sulfite was added and the resulting mixture was separated using methylene chloride (200 ml). The organic layer was dried over anhydrous magnesium sulfate, the filtrate was concentrated and the concentrate was purified by chromatography on a silica gel column (5% methanol—methylene chloride). Petroleum ether was added to the residue. Colorless powder so precipitated was collected by filtration, followed by drying, whereby the title compound (5.47 g) was obtained.

Fuente