反应详情

6.09 g of 1-[(2-methoxy-3-pyridyl)methyl]-4-[2-(3-methylsulfonyl-2-thienyl)ethyl]piperidine obtained in Example 43 and 2 ml of thionyl chloride were dissolved in 50 ml of ethanol, and the mixture was heated under reflux for 2 hours. The reaction mixture was basified by adding a 1N aqueous sodium hydroxide thereto, and then extracted with dichloromethane. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resulting crude product was purified by NH form silica gel column chromatography (ethyl acetate), to give 4.89 g of the title compound as colorless crystals.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 2 hours
3. extractionextracted with dichloromethane
4. washThe organic layer was washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated
7. customthe resulting crude product was purified by NH
8. customform silica gel column chromatography (ethyl acetate)