ethyl 4-oxopiperidine-3-carboxylate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In the same way as described for example 1, 0.3m of 3,4-dimethyl phenol, 0.2m of 3-carbethoxy-4piperidone were reacted to give 8.4g of crude product. Crystallization from ethyl acetate afforded analytical material, m.p. 173°-5° C. were reacted

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In the same way as described for example 1, 0.3m of 3,4-dimethyl phenol, 0.2m of 3-carbethoxy-4piperidone were reacted to give 8.4g of crude product. Crystallization from ethyl acetate afforded analytical material, m.p. 173°-5° C. were reacted

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In the same way as described for example 1, 0.3m of 3,4-dimethyl phenol, 0.2m of 3-carbethoxy-4piperidone were reacted to give 8.4g of crude product. Crystallization from ethyl acetate afforded analytical material, m.p. 173°-5° C. were reacted

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of ethyl 4-oxopiperidine-3-carboxylate (180.0 g, 0.87 mol, 1.0 eq.) in DCM (2.7 L) was added Et3N (352.14 g, 3.48 mol, 4.0 eq.) dropwise at 15° C. and stirred for 30 min followed by addition of (BOC)2O (210.0 g, 0.96 mol, 1.10 eq.) maintaining the temperature below 10° C. The resulted mixture was stirred at rt overnight, and concentrated to give a crude product that was stirred with hexane (3.5 L) for 1 h and filtered. The filtered cake was washed with hexanes. The combined organic phase was concentrated to furnish the title compound (226.0 g, 0.83 mol, 95.4%). maintaining the temperature below 10° C The resulted mixture was stirred at rt overnight concentrated to give a crude product that filtered The filtered cake was washed with hexanes The combined organic phase was concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of ethyl 1-benzyl-4-oxopiperidine-3-carboxylate (360.0 g, 1.21 mol) in EtOH (6.7 L) was added wet Pd/C (55.0 g) under N2 that then was replaced by H2. The reaction mixture was stirred at rt for 4 h, filtered and concentrated to give a crude product. The crude product was slurried with EtOH (200 mL) for 2 h and then filtered. The filtered cake was washed with MTBE and the combined organic phases were concentrated to give the title compound (222.0 g, 1.07 mol, 88.4%). filtered concentrated to give a crude product filtered The filtered cake was washed with MTBE the combined organic phases were concentrated