反应 #2880122
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08637674B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Ethyl 3-oxo-4-phenoxybutanoate (5a, 1.2 g, 5.4 mmol) was charged in a 25 mL round-bottom flask and dissolved in 10 mL of ethanol. A solution of 2-hydrazinopyridine (0.55 g, 5.0 mmol) in 5 mL of ethanol at 100° C. was gradually added thereto over 30 minutes, followed by stirring for 20 hours. After completion of the reaction was confirmed by TLC, the reaction solution was concentrated by evaporation, extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, concentrated, and then purified by column chromatography (n-Hex/EtOAc=9/1 (v/v)) to afford the title compound. the reaction solution was concentrated by evaporation extracted with ethyl acetate washed with saturated brine dried over anhydrous sodium sulfate concentrated purified by column chromatography (n-Hex/EtOAc=9/1 (v/v))
来源 ID: ord-17c8f743babe42f389e89c9fd206f938