反应详情

温度

5 °C

Combine 1-benzyl-4-phenylpiperidine-4-carboxylic acid amide N-oxide (529 g, 1700 mmol), 10% palladium-on-carbon (25 g), and acetic acid (5 L) in an autoclave. Flush the autoclave with nitrogen and then charge with 255 psi of hydrogen. Stir while recharging the autoclave with hydrogen as required to maintain the pressure above 100 psi. When hydrogen consumption ceases, flush the autoclave with nitrogen remove the catalyst by filtration. Evaporate the filtrate invacuo to give a residue. Dissolve the residue in ethyl acetate (5 L), acidify by the addition of 12M aqueous hydrochloric acid solution (150 mL), and heat to reflux for 15 minutes. Cool the mixture to 5° C. to give solid. Collect the solid by filtration, rinse with ethyl acetate, and air dry to give the title compound.

1. customFlush the autoclave with nitrogen
2. additioncharge with 255 psi of hydrogen
3. temperatureto maintain the pressure above 100 psi
4. customWhen hydrogen consumption ceases
5. customflush the autoclave with nitrogen
6. customremove the catalyst
7. filtrationby filtration
8. customEvaporate the filtrate invacuo
9. customto give a residue
10. temperatureheat
11. temperatureto reflux for 15 minutes
12. customto give solid
13. customCollect the solid
14. filtrationby filtration
15. washrinse with ethyl acetate, and air
16. customdry