乙基 (2S)-6-氧代哌啶-2-羧酸乙酯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Absolute ethanol (300 mL) was cooled at −5° C. then thionyl chloride (14.01 mL, 192.1 mmol) was added keeping the temperature below 0° C., followed by portionwise addiction of (S)-6-oxopiperidine-2-carboxylic acid (25.0 g, 174.6 mmol). The mixture was stirred at room temperature for 6 hours. The solvent was evaporated, then toluene (300 mL) and Et3N (48.7 mL) were added. After 0.5 hour the precipitate was filtered and washed with toluene and Et2O. The filtrate was evaporated and the residue treated with Et2O. The precipitate was eliminated and the solution was concentrated to give the title compound as yellow oil. Yield (29.9 g, 100%). the temperature below 0° C. The solvent was evaporated toluene (300 mL) and Et3N (48.7 mL) were added After 0.5 hour the precipitate was filtered washed with toluene and Et2O The filtrate was evaporated the residue treated with Et2O the solution was concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Absolute ethanol (300 mL) was cooled at −5° C. then thionyl chloride (14.01 mL, 192.1 mmol) was added keeping the temperature below 0° C., followed by portionwise addiction of (S)-6-oxopiperidine-2-carboxylic acid (25.0 g, 174.6 mmol). The mixture was stirred at room temperature for 6 hours. The solvent was evaporated, then toluene (300 mL) and Et3N (48.7 mL) were added. After 0.5 hour the precipitate was filtered and washed with toluene and Et2O. The filtrate was evaporated and the residue treated with Et2O. The precipitate was eliminated and the solution was concentrated to give the title compound as yellow oil. Yield (29.9 g, 100%). the temperature below 0° C. The solvent was evaporated toluene (300 mL) and Et3N (48.7 mL) were added After 0.5 hour the precipitate was filtered washed with toluene and Et2O The filtrate was evaporated the residue treated with Et2O the solution was concentrated