Synthesis method for neohesperidin dihydrochalcone
A technology of neohesperidin dihydrochalcone and neohesperidin, which is applied in the field of synthesis of neohesperidin dihydrochalcone, and can solve the problem of high price of catalyst palladium carbon, increase of production cost, increase of operation steps, etc. problems, to achieve the effects of reducing environmental toxicity and production costs, easy operation, and improving safety
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Embodiment 1
[0031] (1) Stir and dissolve 5g of sodium hydroxide in 100mL of a mixed solvent of ethanol and water with a mass ratio of 1:9 and pour it into a 250mL three-neck flask, add 10g of neohesperidin and stir to dissolve, then add 1g of skeleton nickel as a catalyst, Use a nitrogen balloon to exhaust the air in the three-necked flask, and then use a hydrogen balloon to exhaust the nitrogen, so that the reaction is carried out at room temperature under a hydrogen pressure of 0.1MPa for 6 hours, filter out the skeleton nickel, and adjust the pH value of the reaction solution to 7 with hydrochloric acid. , then concentrating the reaction solution to saturation, cooling and crystallizing, and then filtering off the crystals to obtain the crude neohesperidin dihydrochalcone;
[0032] (2) Take 5g of crude neohesperidin dihydrochalcone, add 25mL of deionized water, heat and stir at 85°C to dissolve and cool the crystals for 12 hours, filter out the crystals, wash once with cold ethanol of t...
Embodiment 2
[0034] (1) Take 1kg of sodium hydroxide, stir and dissolve it in 20L of ethanol and water with a mass ratio of 1:9 and pour it into a hydrogenation reactor, add 2kg of neohesperidin and stir to dissolve, then add 200g of skeleton nickel as a catalyst, use Exhaust the air in the reaction kettle with nitrogen, and then exhaust the nitrogen with hydrogen, so that the reaction is carried out at room temperature under the hydrogen pressure of 0.1MPa for 6 hours, filter out the skeleton nickel, adjust the pH value of the reaction solution to 7 with hydrochloric acid, and then react The solution was concentrated to saturation, cooled and crystallized, and then the crystals were filtered off to obtain the crude product of neohesperidin dihydrochalcone;
[0035] (2) Take 1kg of crude neohesperidin dihydrochalcone, add 5L of deionized water, heat and stir at 85°C to dissolve and cool the crystals for 12 hours, filter out the crystals, wash once with cold ethanol of the same quality as th...
Embodiment 3
[0037] (1) Stir and dissolve 10kg of sodium hydroxide in 200L of a mixed solvent of ethanol and water with a mass ratio of 1:9 and pour it into a hydrogenation reactor. Exhaust the air in the reaction kettle with nitrogen, and then exhaust the nitrogen with hydrogen, so that the reaction is carried out at room temperature under the hydrogen pressure of 0.1MPa for 6 hours, filter out the skeleton nickel, adjust the pH value of the reaction solution to 7 with hydrochloric acid, and then react The solution was concentrated to saturation, cooled and placed for crystallization, and then the crystals were filtered out to obtain the crude product of neohesperidin dihydrochalcone, which was freeze-dried to obtain the crude product of neohesperidin dihydrochalcone;
[0038] (2) Take 10kg of crude neohesperidin dihydrochalcone, add 50L of deionized water, heat and stir at 85°C to dissolve and cool the crystals for 12 hours, filter out the crystals, rinse once with cold ethanol of the sam...
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