Preparation method of kaempferol
A technology of kaempferol and hydroxyacetophenone, which is applied in the field of raw drug synthesis, can solve the problems of difficulty in meeting industrial production requirements, large waste of plant resources and solvents, and long synthesis routes, so as to save plant resources and solvents and reduce costs , the effect of short synthetic route
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Embodiment 1
[0034] 1) Hydrolysis prepares hydroxyacetophenone intermediate
[0035] 1.1) 30g of dihydromyricetin with a content of more than 98% is dropped into the reactor, then add 400g of sodium hydroxide solution with a mass fraction of 15%, stir and mix evenly, heat up and reflux, and carry out hydrolysis reaction; high performance liquid chromatography monitoring, with The hydroxyacetophenone intermediate no longer increases as the reaction control end point, and after 2h, the reaction is stopped. Cool down to 30°C, slowly add 50% hydrochloric acid solution dropwise to the reaction solution, adjust the pH to about 6.2, stir for 2 hours, let stand for 1 hour, and filter to obtain a light yellow sticky solid.
[0036] 1.2) Add 150 g of 95% ethanol to the light yellow sticky solid obtained in step 1.1), heat up and reflux for 1 h, then filter while hot to obtain the solid, then add 90 g of 95% ethanol to the solid, heat up and reflux again for beating for 1 h, and Stand at room temper...
Embodiment 2
[0044] 1) Hydrolysis prepares hydroxyacetophenone intermediate
[0045] 1.1) 30g of dihydromyricetin with a content of more than 98% is dropped into the reactor, and then 325g of sodium hydroxide solution with a mass fraction of 17.5% is added, stirred and mixed uniformly, heated and refluxed, and hydrolyzed; monitored by high performance liquid chromatography, with The hydroxyacetophenone intermediate no longer increases as the reaction control end point, and after 2h, the reaction is stopped. Cool down to 30°C, and slowly add 50% hydrochloric acid solution dropwise to the reaction liquid, adjust the pH to about 6.5, stir for 2 h, let stand for 1 h, and filter to obtain a light yellow sticky solid.
[0046] 1.2) Add 145 g of 95% ethanol to the light yellow sticky solid obtained in step 1.1), heat up and reflux for 1 h, then filter while hot to obtain the solid, then add 100 g of 95% ethanol to the solid, heat up and reflux again for beating for 1 h, and Stand at room tempera...
Embodiment 3
[0054] 1) Hydrolysis prepares hydroxyacetophenone intermediate
[0055] 1.1) 30g of dihydromyricetin with a content of more than 98% is dropped into the reactor, then add 210g of sodium hydroxide solution with a mass fraction of 20%, stir and mix evenly, heat up and reflux, and carry out hydrolysis reaction; high performance liquid chromatography monitoring, with The hydroxyacetophenone intermediate no longer increases as the reaction control end point, and after about 1.5h, the reaction is stopped. The temperature was lowered to 30°C, and 50% hydrochloric acid solution was slowly added dropwise to the reaction solution to adjust the pH to about 6.3, stirred for 2 hours, left to stand for 1 hour, and filtered to obtain a light yellow sticky solid.
[0056] 1.2) Add 100 g of 95% ethanol to the light yellow sticky solid obtained in step 1.1), heat up and reflux for 1 h, then filter while hot to obtain the solid, then add 120 g of 95% ethanol to the solid, heat up and reflux agai...
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