反应详情

A mixture of 1.15 g of N-(1-benzyl-4-methylpiperidin-4-yl)-8-(cyclohexylmethoxy)-2-methylimidazolo[1,2-a]pyridine-3-carboxamide, 0.4 mL of 1-chloroethyl chloroformate, and 15 mL of dichloroethane was heated to reflux overnight. After leaving to be cooled at room temperature, the solvent was evaporated under reduced pressure, and to the residue was added 15 mL of methanol, followed by heating to reflux for 6 hours. After leaving to be cooled at room temperature, the solvent was evaporated under reduced pressure, and to the residue were added a saturated aqueous sodium hydrogen carbonate solution and chloroform to carry out a layer separation operation. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 426 mg of 8-(cyclohexylmethoxy)-2-methyl-N-(4-methylpiperidin-4-yl)imidazolo[1,2-a]pyridine-3-carboxamide.

1. temperaturewas heated
2. temperatureto reflux overnight
3. customAfter leaving
4. customthe solvent was evaporated under reduced pressure
5. additionto the residue was added 15 mL of methanol
6. temperatureby heating
7. temperatureto reflux for 6 hours
8. customAfter leaving
9. temperatureto be cooled at room temperature
10. customthe solvent was evaporated under reduced pressure
11. additionto the residue were added a saturated aqueous sodium hydrogen carbonate solution and chloroform
12. customa layer separation operation
13. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
14. customthe solvent was evaporated under reduced pressure
15. customThe residue was purified by silica gel column chromatography