반응 #158348

반응 방정식

ethyl 2-oxopiperidine-3-carboxylate

trimethyloxonium tetrafluoroborate

3-Methoxy-4-(4-methyl-1H-imidazol-1-yl)benzohydrazide

→

title compound

수율 38.2%

ethyl 3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridine-8-carboxylate

수율 38.2%

용매

acetonitrile

ethyl acetate

sodium hydrogen carbonate

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도under reflux for 2 hr
3. 3
   온도to cool to room temperature
4. 4
   세척the mixture was washed with saturated brine
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   기타the solvent was evaporated under reduced pressure
7. 7
   여과The residue was collected by filtration
8. 8
   세척washed with ethyl acetate

실험 절차

To a mixture of ethyl 2-oxopiperidine-3-carboxylate (1.86 g) in acetonitrile (20 mL) was added trimethyloxonium tetrafluoroborate (1.61 g) at room temperature, and the mixture was stirred at room temperature for 2 hr. 3-Methoxy-4-(4-methyl-1H-imidazol-1-yl)benzohydrazide (2.23 g) was added to the reaction mixture at room temperature, and the mixture was heated under reflux for 2 hr. The reaction mixture was allowed to cool to room temperature, and diluted with ethyl acetate and saturated aqueous sodium hydrogen carbonate solution, the mixture was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was collected by filtration, and washed with ethyl acetate to give the title compound (1.32 g).

출처