反应详情

9.6 g of 1-[(2-methoxy-3-pyridyl)methyl]-4-[2-oxo-2-(2-thienyl)ethyl]piperidine obtained in Example 54 and 8.5 ml of thionyl chloride were dissolved in 60 ml of ethanol, and the mixture was heated under reflux for 3 hours. The solvent was evaporated, and then the residue was dissolved in chloroform and a 1N aqueous sodium hydroxide. The organic layer was separated, washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was recrystallized from ethanol, to give 9.0 g of the title compound as colorless crystals.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 3 hours
3. customThe solvent was evaporated
4. dissolutionthe residue was dissolved in chloroform
5. customThe organic layer was separated
6. washwashed with brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was evaporated
9. customthe crude product was recrystallized from ethanol