tert-butyl 2-(4-hydroxypiperidin-1-yl)acetate

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

实验步骤: To a heated (40° C.) solution of tert-butyl 2-bromoacetate (7.38 mL, 49.9 mmol) in THF (10 mL) was added dropwise a solution of piperidin-4-ol (5.050 g, 49.9 mmol) and TEA (6.96 mL, 49.9 mmol) in THF (50 mL). The mixture was refluxed for 2 hours and then cooled to RT and filtered through a pad of Celite® brand filter aid. The filtrate was evaporated and the residue diluted with EtOAc (50 mL), washed with water (50 mL), brine (10 mL), and the organic layer dried over Na2SO4, filtered and evaporated. The material was purified via flash chromatography using a linear gradient of 0% to 10% of 1% NH4OH in MeOH in DCM. The title compound was isolated as an off-white solid (4.865 g, 45% yield). The mixture was refluxed for 2 hours filtered through a pad of Celite® brand filter aid The filtrate was evaporated the residue diluted with EtOAc (50 mL) washed with water (50 mL), brine (10 mL) the organic layer dried over Na2SO4 filtered evaporated The material was purified via flash chromatography

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

实验步骤: To a heated (40° C.) solution of tert-butyl 2-bromoacetate (7.38 mL, 49.9 mmol) in THF (10 mL) was added dropwise a solution of piperidin-4-ol (5.050 g, 49.9 mmol) and TEA (6.96 mL, 49.9 mmol) in THF (50 mL). The mixture was refluxed for 2 hours and then cooled to RT and filtered through a pad of Celite® brand filter aid. The filtrate was evaporated and the residue diluted with EtOAc (50 mL), washed with water (50 mL), brine (10 mL), and the organic layer dried over Na2SO4, filtered and evaporated. The material was purified via flash chromatography using a linear gradient of 0% to 10% of 1% NH4OH in MeOH in DCM. The title compound was isolated as an off-white solid (4.865 g, 45% yield). The mixture was refluxed for 2 hours filtered through a pad of Celite® brand filter aid The filtrate was evaporated the residue diluted with EtOAc (50 mL) washed with water (50 mL), brine (10 mL) the organic layer dried over Na2SO4 filtered evaporated The material was purified via flash chromatography

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

实验步骤: To a heated (40° C.) solution of tert-butyl 2-bromoacetate (7.38 mL, 49.9 mmol) in THF (10 mL) was added dropwise a solution of piperidin-4-ol (5.050 g, 49.9 mmol) and TEA (6.96 mL, 49.9 mmol) in THF (50 mL). The mixture was refluxed for 2 hours and then cooled to RT and filtered through a pad of Celite® brand filter aid. The filtrate was evaporated and the residue diluted with EtOAc (50 mL), washed with water (50 mL), brine (10 mL), and the organic layer dried over Na2SO4, filtered and evaporated. The material was purified via flash chromatography using a linear gradient of 0% to 10% of 1% NH4OH in MeOH in DCM. The title compound was isolated as an off-white solid (4.865 g, 45% yield). The mixture was refluxed for 2 hours filtered through a pad of Celite® brand filter aid The filtrate was evaporated the residue diluted with EtOAc (50 mL) washed with water (50 mL), brine (10 mL) the organic layer dried over Na2SO4 filtered evaporated The material was purified via flash chromatography