Preparation method of 3,5,7,3',4',5'-hexahydroxy flavone
A technology of hexahydroxyflavone and dihydromyricetin is applied in the field of preparation of natural product 3,5,7,3',4',5'-hexahydroxyflavone, and can solve the problems of unsuitability for industrial production, complicated operation and high yield. Low rate and other problems, to achieve the effect of cheap price, simple operation and high yield
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Embodiment 1
[0029] 50 g of dihydrogen genus was added to the high pressure reactor, and 500 ml of pure water was added to the high pressure reaction kettle, and then anhydrous potassium carbonate was added 4.25 g, and 0.25 g of iodine, stirred well, and the oxygen was warmed, and the temperature was 80 ° C. When the pressure is 0.2 MPa, the air is stopped into the oxygen, and the insulation is charged. Sampling after 6 hours, the feedstock reaction is completed, and the reaction is stopped. The reaction liquid was lowered to room temperature, and the pH of the reaction liquid was adjusted with hydrochloric acid, filtered to give a solid, and the solid was dissolved with ethanol, concentrated to a third, filtered to give a yellow solid 39.4 g, and detected by HPLC, such as figure 1 As shown, it is greater than 98%.
Embodiment 2
[0031] 50 g of dihydrofilltraphen was added to the high pressure reactor, and 600 ml of water was added to the high pressure reactor, then anhydrous potassium carbonate was added 4.25 g, 1.5 g of iodine, stirred, and the oxygen was heated, and the temperature reached 100 ° C, pressure of 100 ° C, pressure When 0.2 MPa, the oxygen is stopped, and the insulation is charged. 4 post-hour sampling detection, the feedstock reaction is completed, stop the reaction. The reaction liquid decreased to room temperature, and the pH of the reaction liquid was adjusted with hydrochloric acid, filtered, the solid was dissolved with ethanol, concentrated to one-third, and filtered to give a yellow solid 41.5 g. Test by HPLC, such as figure 2 As shown, it is greater than 98%.
Embodiment 3
[0033] 50 g of dihydrogen genus was added to the high pressure reactor, and 500 ml of water was added to the high pressure reaction kettle, 4.25 g of anhydrous carbonate was added, 0.5 g of iodine, stirred, and the oxygen was heated, and the temperature was 100 ° C, and the pressure was When 0.25MPa, the oxygen is stopped, and the holding pressure reactions are charged. 5 After hours of sampling detection, the feedstock reaction was completed, and the reaction was stopped. The reaction liquid decreased to room temperature, and the pH of the reaction liquid was adjusted with hydrochloric acid to be filtered, and the solid was purified to give a yellow solid 41.3 g. Through HPLC detection, the Yangmei content is greater than 98%.
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