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CAS No. : | 2306-27-6 | MDL No. : | MFCD00017421 |
Formula : | C20H20O7 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | LKMNXYDUQXAUCZ-UHFFFAOYSA-N |
M.W : | 372.37 | Pubchem ID : | 145659 |
Synonyms : |
Pedalitin permethyl ether
|
Chemical Name : | 2-(3,4-Dimethoxyphenyl)-5,6,7-trimethoxy-4H-chromen-4-one |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P302+P352-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; ethanol; at 80℃; for 18 - 70h;Heating / reflux;Product distribution / selectivity; | 54 g of the above obtained fraction were refluxed in 500 ml of a HCl solution in ethanol (1.25 M, Fluka) for 70 h. The ethanol was evaporated. About 100 ml of fresh ethanol <n="8"/>were added and evaporated to dryness. This was repeated two times. 46.5 g of 5-hydroxy polymethoxyflavones-rich fraction were obtained. This fraction contained at least 85% w/w of 5-desmethyl polymethoxyflavones, relative to total flavone fraction (HPLC- UV-MS). Further HPLC purification work and NMR analyses showed the presence of 5-desmethylsinensetin, 5-desmethyl<strong>[478-01-3]nobiletin</strong>, 5-desmethyltangeretin, 5-desmethyl-TOM- scutellarein, 5-desmethyl-HOM-quercetagenin and 5-hydroxy-3,6,7,8,34'- hexamethoxyflavone; 300 mg of a polymethoxyflavone-rich extract obtained in Example 3 were reacted at 8O0C in the presence of ethanolic HCl solutions having different amounts of water. All the different experiments were analysed by HPLC after 18 hours of reaction to monitor the progression. The results (UV-peak area) are shown in Table 1 hereinbelow: | |
With hydrogenchloride; ethanol; water; at 80℃; for 18h;Heating / reflux;Conversion of starting material; | The same result was obtained in 1.6 ml of ethanol and 0.4 ml of concentrated HCl; 300 mg of a polymethoxyflavone-rich extract obtained in Example 3 were reacted at 8O0C in the presence of ethanolic HCl solutions having different amounts of water. All the different experiments were analysed by HPLC after 18 hours of reaction to monitor the progression. The results (UV-peak area) are shown in Table 1 hereinbelow: <n="9"/>PMF: polymethoxyflavoneAs it can be seen easily, if the water content of the alcoholic HCl solution is above 50% w/w, the yield of conversion is very low and preferably said water content should be below 33% or 20%. | |
With ethanol; water; for 24h;Heating / reflux;Product distribution / selectivity; | 165 mg of the PMF rich fraction were refluxed over 24 hours in 1.8 ml of ethanol and 0.2 ml of concentrated aqueous. About 15 ml of water were added and the mixture was extracted two times with 5 ml of dichloromethane. The organic phase was dried over Na2SO4 and the solvent was evaporated. 124 mg (yield: 75%) of 5-hydroxy polymethoxyflavones-rich fraction were obtained. This fraction contained a proportion of 5-desmethyl polymethoxyflavones, relative to total flavones, higher than 95 % (HPLC- UV-MS). |