反应 #1606709
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08946296B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a suspension of K2CO3 (3.48 g, 25.4 mmol, 2.1 equiv) in dry DMF (30 mL) a solution of (trans)-2-(4-bromophenyl)cyclopropanamine hydrochloride (3 g, 12.09 mmol, 1 equiv) in dry DMF (6 mL) was added at 0° C. and stirred for 10 min, then 2-bromoacetamide (1.82 g, 13.3 mmol, 1.1 equiv) was added and stirred at RT for 2 h. After completion, the reaction mixture was poured into ice water (50 mL) and extracted with EtOAc (2×50 mL). The combined extracts were washed with water (2×50 mL), brine (50 mL), dried over anhydrous Na2SO4, filtered and evaporated. The crude residue was purified by column chromatography (SiO2) using MeOH:CHCl3 (3:97) to get 2-((trans)-2-(4-bromophenyl)cyclopropylamino)acetamide (1 g, 31% yield) as a white solid. was added at 0° C. stirred at RT for 2 h extracted with EtOAc (2×50 mL) The combined extracts were washed with water (2×50 mL), brine (50 mL) dried over anhydrous Na2SO4 filtered evaporated The crude residue was purified by column chromatography (SiO2)
来源 ID: ord-bb9c0844309a4cc584bc4fbbdda244b1