反应详情

To a solution of 5.8 g of 3-(cyclohexylmethoxy)pyridin-2-amine in 100 ml of toluene were added 4.3 ml of ethyl 2-chloro-3-oxobutanoate and 4.3 ml of triethylamine, followed by stirring overnight under heating to reflux. To the reaction mixture were added 1 ml of ethyl 2-chloro-3-oxobutanoate and 1 ml of triethylamine, followed by stirring for 6.5 hours under heating to reflux. To the reaction mixture was added water, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and the solvent was then evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography. To the purified product thus obtained were added ethyl acetate and hexane, followed by heating and stirring, and then stirring under ice-cooling. The resulting solid was collected by filtration to obtain 4.0 g of ethyl 8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridine-3-carboxylate.

1. temperatureunder heating to reflux
2. stirringby stirring for 6.5 hours
3. temperatureunder heating to reflux
4. extractionfollowed by extraction with ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. customthe solvent was then evaporated under reduced pressure
7. customThe obtained residue was purified by silica gel column chromatography
8. customTo the purified product thus obtained
9. temperatureby heating
10. stirringstirring
11. stirringstirring under ice-
12. temperaturecooling
13. filtrationThe resulting solid was collected by filtration