Reacción #633964

Ecuación de reacción

Trifluoroacetic acid

ammonium acetate

N-(2,6-difluoropyridin-3-yl)-N-(2-oxopropyl)formamide

sodium bicarbonate

→

title compound

Rendimiento 95.4%

2,6-difluoro-3-(4-methyl-1H-imidazol-1-yl)pyridine

Rendimiento 95.4%

Disolventes

toluene

ethyl acetate

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturathe reaction solution was heated
2. 2
   Temperaturaunder reflux in a nitrogen atmosphere for four hours
3. 3
   OtroAfter leaving
4. 4
   Temperaturato cool
5. 5
   Otrothe organic layer was separated
6. 6
   LavadoThe resulting organic layer was washed with brine
7. 7
   Secadodried over anhydrous sodium sulfate
8. 8
   OtroThe drying agent was separated by filtration
9. 9
   Concentraciónthe organic layer was concentrated under reduced pressure
10. 10
    OtroThe residue was purified by silica gel column chromatography

Procedimiento

Trifluoroacetic acid (1.08 ml) and ammonium acetate (1.08 g) were added to a solution of N-(2,6-difluoropyridin-3-yl)-N-(2-oxopropyl)formamide (2.52 g) in toluene (40 ml), and the reaction solution was heated under reflux in a nitrogen atmosphere for four hours. After leaving to cool, ethyl acetate and a saturated sodium bicarbonate solution were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and then the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (2.19 g). The property values of the compound are as follows.

Fuente