O, o'-dialkyl-o"-(substituted flavone-3-yl) phosphate derivatives, preparation method and application
A phosphate ester, dimethoxyflavonoid technology, applied in the fields of botanical equipment and methods, chemicals for biological control, applications, etc. The effect of multiple reaction sites
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Embodiment 1
[0043] O, the preparation method of O'-diethyl-O "-(4'-fluoro-7-methoxyflavone-3-yl) phosphate ester (compound number is A1), comprises the following steps:
[0044] (1) Preparation of 2-hydroxyl-4-methoxyacetophenone
[0045] Add raw materials 2,4-dihydroxyacetophenone (3.29mmol), 30mL acetonitrile and (4.93mmol) anhydrous potassium carbonate into a 50mL single-necked flask, stir at room temperature for 0.5h, then add iodomethane (3.61mmol), TLC monitoring to the raw material After disappearing, stop the reaction, extract with ethyl acetate, and distill under reduced pressure to obtain a crude product, which is subjected to silica gel column chromatography [V (petroleum ether): V (ethyl acetate) = 10: 1] to obtain 2-hydroxy-4-methoxy Acetophenone, yield 90%.
[0046] (2) Preparation of 4-fluoro-2'-hydroxy-4'-methoxychalcone
[0047] Add 30ml of 20% (V / V) ethanol and (11.06mmol) sodium hydroxide in a 50mL single-necked flask, stir at room temperature for 0.5h, then add subst...
Embodiment 2
[0053] O, the preparation method of O'-diethyl-O "-(3'-bromo-7-methoxyflavone-3-yl) phosphate ester (compound number is A2), comprises the following steps:
[0054] (1) Preparation of 2-hydroxyl-4-methoxyacetophenone:
[0055] As in the first (1) step of Example 1.
[0056] (2) Preparation of 3-bromo-2'-hydroxyl-4'-methoxychalcone:
[0057] As in the (2) step of Example 1, the difference is that 3-bromobenzaldehyde is used as a raw material.
[0058] (3) Preparation of 3'-bromo-7-methoxyflavonol:
[0059] As in step (3) of Example 1, the difference is that 3-bromo-2'-hydroxyl-4'-methoxyl group is used as raw material.
[0060] (4) Preparation of O, O'-diethyl-O"-(3'-bromo-7-methoxyflavone-3-yl) phosphate ester:
[0061] As in the (4) step of Example 1, the difference is that 3'-bromo-7-methoxyflavonol is used as a raw material. The yield is 65%, and the melting point is 80-82°C.
Embodiment 3
[0063] O, the preparation method of O'-diethyl-O "-(7-methoxyflavone-3-yl) phospholipid (compound number is A3), comprises the following steps:
[0064] (1) Preparation of 2-hydroxyl-4-methoxyacetophenone:
[0065] As in the first (1) step of Example 1.
[0066] (2) Preparation of 2'-hydroxyl-4'-methoxychalcone:
[0067] As in the (2) step of embodiment 1, the difference is that benzaldehyde is used as a raw material.
[0068] (3) Preparation of 7-methoxyflavonol:
[0069] As in step (3) of Example 1, the difference is that 2'-hydroxyl-4'-methoxychalcone is used as a raw material.
[0070] (4) Preparation of O, O'-diethyl-O"-(7-methoxyflavone-3-yl) phosphate ester:
[0071] As in step (4) of Example 1, the difference is that 7-methoxyflavonol is used as a raw material. Yield 52%, melting point 72-74°C.
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