反应详情

20.3 g of 1-benzyl-4-(2,3-methylenedioxyphenethyl)piperidine was dissolved in 10 ml of 1,2-dichloroethane, 7 ml of 1-chloroethyl chloroformate was added thereto under ice-cooling, and the mixture was heated under reflux for 30 minutes. The solvent was evaporated, the resulting residue was dissolved in 100 ml of methanol, and the mixture was heated under reflux for one hour. The solvent was removed, the resulting residue was basified by adding a 5N aqueous sodium hydroxide, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified by NH form silica gel column chromatography (ethyl acetate), to give 13.1 g of the title compound as a pale yellow oil.

1. temperatureunder ice-cooling
2. temperaturethe mixture was heated
3. temperatureunder reflux for 30 minutes
4. customThe solvent was evaporated
5. dissolutionthe resulting residue was dissolved in 100 ml of methanol
6. temperaturethe mixture was heated
7. temperatureunder reflux for one hour
8. customThe solvent was removed
9. additionby adding a 5N aqueous sodium hydroxide
10. extractionthe mixture was extracted with ethyl acetate
11. washThe organic layer was washed with brine
12. dry with materialdried over anhydrous magnesium sulfate
13. customThe solvent was evaporated
14. customthe crude product was purified by NH
15. customform silica gel column chromatography (ethyl acetate)