反应 #3403007
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08716309B2
反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: After 1.24 g (6.1 mmol) of dimethyl 4-(methoxymethylene)2-pentenedioate obtained in Example 1-1 was dissolved in 10 mL of DMF, 830 g (6.1 mmol) of 4-dimethylaminoaniline was added to the solution. Afterward, the resulting reaction solution was stirred under reflex at about 50° C. for about 3 hours. After termination of the reaction was determined by liquid chromatography, the solvent was removed in vacuo and was then washed using brine, followed by drying using magnesium sulfate and filtration. After distillation under reduced pressure, the resulting product was purified using column chromatography (hexane:ethyl acetate=1:1) to obtain a target compound (Actual yield: 357 mg, Yield ratio: 21%). Afterward, the resulting reaction solution the solvent was removed in vacuo was then washed by drying magnesium sulfate and filtration After distillation under reduced pressure the resulting product was purified to obtain a target compound (Actual yield: 357 mg, Yield ratio: 21%)
来源 ID: ord-e702e65d08a74266a6baf9ced7c06115