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methyl 2-(4-oxocyclohexylidene)propanoate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In toluene; at 100℃;
A mixture of methyl 2-(triphenylphosphoranylidene)propanoate (2.5 g, 7.18 mmol) and cyclohexane-1,4-dione (1.609 g, 14.35 mmol) in toluene (25 mL) was stirred at 100 C. overnight and then concentrated in vacuo. The residue was triturated with a mixture of hexanes (100 mL) and ethyl acetate (100 mL), and filtered. The filtrate was concentrated in vacuo and the residue was purified by flash chromatography on Analogix IntelliFlash280 eluting with 0 to 50% ethyl acetate/hexanes to provide the title compound. 1H NMR (400 MHz, DMSO-d6) δ 1.85 (p, J=1.5 Hz, 3H), 2.27-2.35 (m, 2H), 2.41 (dd, J=8.0, 5.8 Hz, 2H), 2.55-2.65 (m, 2H), 2.81-2.90 (m, 2H), 3.66 (s, 3H).
General procedure: The p-benzoquinone (0.096 mol) was dissolved in 100 mL of 1,2-dichloroethane, heated to 60 C., stirred until dissolution was complete, compound A-1 was added dropwise, and the reaction was completed by refluxing for 8 h.The reaction solution was allowed to naturally cool to room temperature and allowed to stand overnight to precipitate a solid, which was filtered by suction, washed with cold acetone, dried, and recrystallized from acetone to obtain compound A-2. Yield: 40-60%.
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