Semi-synthesis method of phenolic hydroxyl flavonoid compounds and iodine recycling method
A technology of phenolic hydroxyflavonoids and phenolic hydroxy dihydroflavonoids is applied in the fields of medicine and chemistry, and can solve the problems of large amount of pyridine, low product yield, cumbersome post-processing and the like
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Embodiment 1
[0035] Take 5g of 95% hesperetin in a 250ml iodine measuring bottle, add 6ml of pyridine, 20ml of ethylene glycol and 4.2g of iodine, stir well, and react in a sealed water bath at 80°C (or a drying tube with calcium chloride added to the upper end of the condenser tube). Stir once every 1 hour, after 2 hours, it becomes a homogeneous liquid, and continue to seal the reaction for 6 hours. Add 0.5g of sodium hydrosulfite, stir evenly, quickly pour into 300ml of 1.5% NaOH solution, stir to dissolve, add hydrochloric acid to make it acidic, place it in a closed place for 30min, and then filter with suction to obtain acid water solution 1 (stored in a separate container) and filter cake . Wash the filter cake with water until there is no acidity, dissolve the filter cake with 50% ethanol alkaline water, adjust the pH to 3-5 with hydrochloric acid, and filter after standing for 3 hours, wash the filter cake with a small amount of 50% ethanol, and dry it at 60°C, that is Obtain 4.6...
Embodiment 2
[0038] Take 5g of 95% hesperetin in a 250ml iodine measuring bottle, add 6ml of 2-methylpyridine, 20ml of glycerol and 4.2g of iodine, stir well, and react in a closed water bath at 85°C (or add calcium chloride to the upper end of the condenser tube to dry tube), stir once, after 1 hour it becomes a homogeneous liquid, continue the closed reaction for 7 hours, add 0.5g of sodium hydrosulfite, stir evenly, quickly pour into 300ml of 1.5% NaOH solution, stir to dissolve, quickly add phosphoric acid to adjust to acidity, stir, After airtight for 30 minutes, filter with suction to obtain acid water solution 2 (stored in a separate container) and filter cake. Wash the filter cake with water until it is acid-free, wash the filter cake with a small amount of 50% ethanol, and dry it at 60°C to obtain 4.68g of diosmin with a purity of 96.5%.
Embodiment 3
[0040] Take 10g of 98% naringin in a 250ml iodine measuring bottle, add 5ml of 2-methylpyridine, 20ml of glycerin and 4.3g of iodine, stir well, and react in a water bath at 80°C (or add calcium chloride to the upper end of the condenser tube for drying). tube), stir once every 2 hours, after 8 hours it becomes a homogeneous liquid, add 0.5g of sodium hydrosulfite, stir evenly, quickly pour into 500ml aqueous solution, stir to dissolve, add phosphoric acid to make it acidic, seal it for 5 hours, and suction filter to get Acid water 3 (storage in another container) and filter cake. Wash the filter cake with water until it is acid-free, soak the filter cake with a small amount of 50% ethanol to wash the filter cake, and dry it at 60°C to obtain 8.89 g of Rhodoglucoside with a purity of 98.9%.
[0041]
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