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1-(4-ethoxyphenyl)-3-(2-methoxyphenyl)propane-1,3-dione[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
31.8%
With sodium hydride; In tetrahydrofuran; mineral oil;Reflux;
General procedure: To a suspension of sodium hydride (60% in mineral oil, 5 eq) in dryTHF was added solution of substituted methyl benzoate (2 eq) in dryTHF. After mixture refluxed, substituted acetophenone (1 eq) in dryTHF was added dropwise. The mixture was refluxed overnight, then quenched with 1 N HCl. The mixture was extracted with ethyl acetatetwice, and the combined organic phase was washed with brine solution,dried with anhydrous Na2SO4, filtrated, and concentrated under reduced pressure. The residue was purified on a silica gel column.
(2Z,4E)‑2‑cyano‑3,5‑bis(methylsulfanyl)‑5‑(2‑methoxyphenyl)penta‑2,4‑dienoic acid amide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
34%
With sodium hydroxide; In dimethyl sulfoxide; at 20℃;
General procedure: To a solution of 3,3-bis(methylsulfanyl)methylenemalononitrile 1 (1.70 g, 10 mmol) in 20 mL of DMSO, keton 2a - j (10 mmol) and powdered sodium hydroxide (0.8 20 mmol) were added, and the mixture was magnetically stirred for 4 - 5 h at room temperature. After addition of 300 mL of water to the mixture, the solution was stirred for 12 h at room temperature. The formed precipitate was collected by filtra- tion and washed several times with water. After drying under air, the formed product was recrystallized using methanol or ethanol to obtain the pure products.
Chemistry
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Material Science
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120K+ Compounds
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