反应详情

1-Benzyl-4-(4-fluoro-phenyl)-piperidine-4-carboxylic acid amide N-oxide (5.3 g, 16.3 mmol) and 10% palladium-on-carbon (0.6 g) and acetic acid (100 mL) were combined in a pressure vessel. The reaction mixture was treated with hydrogen on a Parr apparatus at an initial pressure of 53 psi of hydrogen. When hydrogen consumption stopped the catalyst was removed by filtration. The filtrate was evaporated in vacuo to give a residue. The residue was dissolved in ethyl acetate (150 mL), acidified by the addition of 12M aqueous hydrochloric acid solution (5 mL), and heated to reflux for 10 minutes. The mixture was cooled to ambient temperature to give a solid which was collected by filtration, rinsed with ethyl acetate, recrystallized from methanol/ethyl acetate to give the title compound.

1. customWhen hydrogen consumption
2. customwas removed by filtration
3. customThe filtrate was evaporated in vacuo
4. customto give a residue
5. temperatureheated
6. temperatureto reflux for 10 minutes
7. customto give a solid which
8. filtrationwas collected by filtration
9. washrinsed with ethyl acetate
10. customrecrystallized from methanol/ethyl acetate