反应 #3333183
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09296722B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a stirred solution of 1,2,2,6,6-pentamethylpiperidin-4-one (1.5 g, 8.88 mmol) in diethyl ether (25 mL) at rt was added MeLi (1.6 M, 5.5 mL, 8.88 mmol) slowly. The resulting mixture was stirred at rt for 30 min before it was quenched with sat. NH4Cl (15 mL). The mixture was then partitioned between EtOAc (35 mL) and sat. NaHCO3 (25 mL). The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure to give crude 1,2,2,4,6,6-hexamethylpiperidin-4-ol (1.51 g) as an oil. LC-MS (ESI) m/z 186 (M+H)+. was quenched with sat. NH4Cl (15 mL) The mixture was then partitioned between EtOAc (35 mL) and sat. NaHCO3 (25 mL) The organic layer was dried over Na2SO4 filtered concentrated under reduced pressure
来源 ID: ord-ea26526e8fa845b3913bf6b5c67a73ea