反应详情

To a suspension prepared from 3.00 g (39.5 mmol) of 50% lithium aluminum hydride in oil and 100 ml of dry THF and maintained at 0° was added dropwise a solution of 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-methylaminoacetyl}-4-(3-chlorophenoxy)piperidine oxalate in 100 ml of dry THF. The mixture was heated at reflux under nitrogen for 12 hours, allowed to cool to room temperature and subsequently cooled in an ice bath. To the mixture was added slowly, dropwise 3 ml of water followed by 3 ml of 15% sodium hydroxide and 9 ml of water. The suspension was filtered and washed with 150 ml of THF, and the THF was evaporated. The residue was extracted with ether, washed with saturated sodium chloride and dried over potassium carbonate. The yield of the dihydrochloride was 9.36 g (79%). Crystallization from ethanol provided analytically pure material.

1. temperaturemaintained at 0°
2. temperatureThe mixture was heated
3. temperatureat reflux under nitrogen for 12 hours
4. temperaturesubsequently cooled in an ice bath
5. additionTo the mixture was added slowly
6. filtrationThe suspension was filtered
7. washwashed with 150 ml of THF
8. customthe THF was evaporated
9. extractionThe residue was extracted with ether
10. washwashed with saturated sodium chloride
11. dry with materialdried over potassium carbonate
12. customCrystallization from ethanol
13. customprovided analytically pure material