反应 #1882052
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09067922B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 4-acetylphenyl acetate (250 mg, 1.4 mmol) in anhydrous THF (5 mL) cooled to −10° C. under nitrogen was added 3M methylmagnesium chloride solution in THF (2.81 mL, 8.42 mmol) over 10 minutes, keeping the internal temperature below −5° C. The resulting pale yellow solution was allowed to warm to room temperature for 5 hours. The reaction mixture was cooled in an ice bath and quenched with saturated aqueous ammonium chloride solution (20 mL). The resulting clear solution was extracted with EtOAc (2×50 mL). The combined organic extracts were washed with brine (50 mL), dried over MgSO4, filtered and concentrated in vacuo. The solid residue was purified by silica gel column chromatography eluting with 10-50% EtOAc in heptanes to afford the title compound as white solid (100 mg, 47%). the internal temperature below −5° C The reaction mixture was cooled in an ice bath quenched with saturated aqueous ammonium chloride solution (20 mL) The resulting clear solution was extracted with EtOAc (2×50 mL) The combined organic extracts were washed with brine (50 mL) dried over MgSO4 filtered concentrated in vacuo The solid residue was purified by silica gel column chromatography eluting with 10-50% EtOAc in heptanes
来源 ID: ord-8582f803d4ea487799aa8657fb520c0e