反应详情

To a solution of 32 mg of N-[(6-chloropyridin-3-yl)methyl]-8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridine-3-carboxamide in 0.6 ml of N-methyl-2-pyrrolidone was added 0.05 ml of ethyl piperidine-4-carboxylate to carry out a reaction at 150° C. for 30 minutes and further at 200° C. for 30 minutes under microwave irradiation. 24 mg of potassium carbonate was added thereto to carry out a reaction at 240° C. for 2 hours under microwave irradiation. To the reaction mixture were added a saturated aqueous ammonium chloride solution and ethyl acetate to carry out a layer separation operation. The organic layer was washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography. To the obtained purified product were added hexane and isopropyl ether, and the resulting solid was collected by filtration and dried to obtain 14 mg of 1-{4-[({[8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridin-3-yl]carbonyl}amino)methyl]pyridin-2-yl}piperidine-4-carboxylic acid.

1. customa reaction at 150° C. for 30 minutes
2. customfurther at 200° C. for 30 minutes under microwave irradiation
3. customa reaction at 240° C. for 2 hours
4. customunder microwave irradiation
5. customa layer separation operation
6. washThe organic layer was washed with water and saturated brine
7. dry with materialdried over anhydrous sodium sulfate
8. customThe solvent was evaporated under reduced pressure
9. customthe obtained residue was purified by silica gel column chromatography
10. customTo the obtained purified product
11. additionwere added hexane and isopropyl ether
12. filtrationthe resulting solid was collected by filtration
13. customdried