A kind of synthetic method of aryl ketocoumarin derivative
A synthetic method and alkyl technology, applied in the synthesis of ketone compounds, organic chemical synthesis, and the synthesis of aryl ketocoumarin derivatives, to achieve the effect of wide industrial application value and good product yield
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Embodiment 1
[0041]
[0042]At room temperature, add 100 mmol of the above formula (I) compound, 150 mmol of the above formula (II) compound, 4 mmol of the catalyst (3 mmol of trifluoro A mixture of copper acetate and 1mmol 1,1'-bis(diphenylphosphino)ferrocene), 100mmol oxidant Na 2 S 2 o 8 , 10mmol reaction auxiliary 1,3-bis(1-adamantyl)imidazolium tetrafluoroborate and 100mmol base triisopropanolamine; then the temperature was raised to 60°C, and the reaction was stirred at this temperature for 8 hours.
[0043] After the reaction, the reaction mixture was filtered while it was hot, the filtrate was naturally cooled to room temperature, then the pH value was adjusted to neutrality, then deionized water was added to fully shake, and finally ethyl acetate was added to extract 2-3 times, the organic phases were combined, and the pH was reduced. concentrated under reduced pressure, and the resulting residue was subjected to silica gel flash column chromatography, and a mixed solvent of ...
Embodiment 2
[0047]
[0048] At room temperature, add 100 mmol of the above formula (I) compound, 200 mmol of the above formula (II) compound, 6 mmol of the catalyst (4.8 mmol tri A mixture of copper fluoroacetate and 1.2mmol 1,1'-bis(diphenylphosphino)ferrocene), 120mmol oxidant Na 2 S 2 o 8 , 20mmol reaction auxiliary 1,3-bis(1-adamantyl)imidazolium tetrafluoroborate and 120mmol base triisopropanolamine; then the temperature was raised to 80°C, and the reaction was stirred at this temperature for 5 hours.
[0049] After the reaction, the reaction mixture was filtered while it was hot, the filtrate was naturally cooled to room temperature, then the pH value was adjusted to neutrality, then deionized water was added to fully shake, and finally ethyl acetate was added to extract 2-3 times, the organic phases were combined, and the pH was reduced. Concentrate under reduced pressure, and the resulting residue is subjected to silica gel flash column chromatography, using a mixed solvent o...
Embodiment 3
[0053]
[0054] At room temperature, add 100 mmol of the above formula (I) compound, 180 mmol of the above formula (II) compound, 8 mmol of the catalyst (6 mmol of trifluoro A mixture of copper acetate and 2mmol 1,1'-bis(diphenylphosphino)ferrocene), 150mmol oxidant Na 2 S 2 o 8 , 15mmol reaction auxiliary 1,3-bis(1-adamantyl)imidazolium tetrafluoroborate and 140mmol base triisopropanolamine; then the temperature was raised to 70°C, and the reaction was stirred at this temperature for 6 hours.
[0055] After the reaction, the reaction mixture was filtered while it was hot, the filtrate was naturally cooled to room temperature, then the pH value was adjusted to neutrality, then deionized water was added to fully shake, and finally ethyl acetate was added to extract 2-3 times, the organic phases were combined, and the pH was reduced. Concentrate under reduced pressure, and subject the obtained residue to flash column chromatography on silica gel, using a mixed solvent of ac...
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