Styrene pyridine compound, its preparation method and use
A technology of styrylpyridine and compound, which is applied in the field of styrylpyridine compound, its preparation and use, can solve the problems of many toxic and side effects, single action target, complex pathogenesis and the like
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Embodiment 1
[0031] When Ar represents the structural unit (B), the general method for preparing styrene pyridine compound (I-1)
[0032] Add 4.0 mmol 5-(chloromethyl)-2,2,8-trimethyl-4 to the reaction flask H -[1,3] dioxane [4,5-c] pyridine (1) and 25.0 mmol of triethyl phosphite, heated and refluxed and stirred for 4.0 hours (reaction progress is tracked by TLC); after the reaction, the pressure is reduced The excess triethyl phosphite was evaporated, and the residue was purified by silica gel column chromatography (eluent: petroleum ether-ethyl acetate=1:1 v / v) to obtain 2,2,8-trimethyl-4 H -[1,3]dioxane[4,5-c]pyridine-5-methyl diethyl phosphate (2), the yield is 95.0%;
[0033] The 2,2,8-trimethyl-4 obtained in the previous step H -[1,3]Dioxane[4,5-c]pyridine-5-methyl diethyl phosphate (2) dissolved in 20 ml of tetrahydrofuran, cooled to 0~5℃, added 10.0 mmol of sodium hydride , Keep stirring and react for 30 minutes, then add benzaldehyde compound (R 1 R 2 PhCHO) 4.0 mmol, keep stirring at...
Embodiment 2
[0039] When Ar represents (A) structural unit, the general method for preparing styrene pyridine compound (I-2)
[0040] Add 4.0 mmol 5-(bromomethyl)-2,2,8-trimethyl-4 to the reaction flask H -[1,3]dioxane[4,5-c]pyridine (1), 10.0 mmol trimethyl phosphite and 25 ml chlorobenzene, heated and refluxed and stirred for 5.0 hours (reaction progress is tracked by TLC); After completion, the excess trimethyl phosphite and chlorobenzene were evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: petroleum ether-ethyl acetate = 1:1 v / v) to obtain 2,2 ,8-Trimethyl-4 H -[1,3]Dioxane[4,5-c]pyridine-5-methyl dimethyl phosphate (2), the yield is 88.2%;
[0041] The 2,2,8-trimethyl-4 obtained in the previous step H -[1,3]Dioxane[4,5-c]pyridine-5-methyl dimethyl phosphate (2) dissolve in 20 ml of toluene, cool to 0~5℃, add 10.0 mmol sodium methoxide , The reaction was stirred at room temperature for 30 minutes, and then benzaldehyde compounds ...
Embodiment 3
[0045] Example 3 General method for preparing salt of styrene pyridine compound (I) and acid
[0046] Add 2.0 mmol of the styrene pyridine compound (I) obtained in the above example 1 or 2 and 50 ml of methanol into the reaction flask, stir evenly, add 6.0 mmol of the corresponding acid, heat and reflux and stir for 10 minutes, and cool after the reaction is complete At room temperature, the solvent was evaporated under reduced pressure, the residue was recrystallized with acetone, and the precipitated solid was filtered to obtain the salt of styrene pyridine compound (I). Its chemical structure was 1 Confirmed by H NMR and ESI-MS.
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