反应 #1798687
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08278319B2
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 tert-butyl 4,4-bis(2-hydroxyethyl)piperidine-1-carboxylate (500 mg, 1.83 mmol) in DCM (10 ml) were added mesyl chloride (0.33 ml, 4.2 mmol) and TEA (1 ml, 7.32 mmol) at −20° C. and the mixture was stirred for 30 min maintaining the same temperature. TLC revealed completion of the reaction and it was quenched with water and extracted with DCM. The organic phase was washed with brine, dried over Na2SO4 and concentrated to dryness. The crude product was purified by column chromatography (silica (100-200), EtOAc-hexane (30%)) to yield the desired compound. Yield: 70% maintaining the same temperature completion of the reaction and it was quenched with water extracted with DCM The organic phase was washed with brine dried over Na2SO4 concentrated to dryness The crude product was purified by column chromatography (silica (100-200), EtOAc-hexane (30%))
来源 ID: ord-a3daa622fbee433aa44d978018aa60b0