Preparation method of neohesperidin dihydrochalcone

A technology of neohesperidin dihydrochalcone and neohesperidin is applied in the field of preparation of neohesperidin dihydrochalcone, and can solve the problem of low purity and yield of neohesperidin dihydrochalcone , higher equipment and technical requirements, increased operation steps, etc., to achieve the effect of easy reuse, lower production costs, and fewer operation steps

Active Publication Date: 2016-10-12
SUZHOU YOUDAN INTERNET TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the traditional process of neohesperidin dihydrochalcone, the hydrogen pressure is high, which not only increases the difficulty of the process, but also reduces the safety. In addition, high temperature and high pressure are generally used in the process of hydrogenation, which requires high equipment and technology. Facilitate operation, and risk is bigger, disclose a kind of synthetic method of neohesperidin dihydrochalcone as patent document CN103804439A; Decolorization increases the operation steps and also brings the risk of introducing impurities in the operation. In addition, the purity and yield of neohesperidin dihydrochalcone obtained by traditional processes are relatively low

Method used

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  • Preparation method of neohesperidin dihydrochalcone

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Embodiment 1

[0028] A preparation method for neohesperidin dihydrochalcone, comprising the following steps:

[0029] Step 1, adding 1kg neohesperidin and 15kg mass fraction of 6% sodium hydroxide solution into the reactor, stirring and dissolving, then adding 0.05kg catalyst palladium carbon, sealing the reactor, replacing the air in the reactor with nitrogen, Then feed hydrogen to replace nitrogen at normal temperature, stir and react under normal pressure for 10 hours, after the reaction is completed, use nitrogen to replace hydrogen in the reactor, then stop the reaction, and extract the reaction solution;

[0030] Step 2, adjust the pH of the reaction solution to 5, crystallize at room temperature for 10 hours, and filter to obtain crystal A; the obtained filtrate is adsorbed with macroporous resin D101, and after adsorption, it is eluted with purified water to remove the salt in the filtrate; then use 15 The volume fraction of twice the column volume is eluted with 10% ethanol, and th...

Embodiment 2

[0032] A preparation method for neohesperidin dihydrochalcone, comprising the following steps:

[0033] Step 1, adding 1kg neohesperidin and 20kg mass fraction of 15% sodium hydroxide solution into the reactor, stirring and dissolving, then adding 0.06kg catalyst palladium carbon, sealing the reactor, replacing the air in the reactor with nitrogen, Then feed hydrogen to replace nitrogen at normal temperature, stir and react under normal pressure for 15 hours, after the reaction is completed, use nitrogen to replace hydrogen in the reactor, then stop the reaction, and extract the reaction solution;

[0034]Step 2. Adjust the pH of the reaction solution to 6, crystallize at room temperature for 15 hours, and filter to obtain crystal A; the obtained filtrate is adsorbed with macroporous resin D101, and after adsorption, it is eluted with purified water to remove the salt in the filtrate; The volume fraction of twice the column volume is eluted with 25% ethanol, and then eluted wi...

Embodiment 3

[0036] A preparation method for neohesperidin dihydrochalcone, comprising the following steps:

[0037] Step 1, adding 1kg neohesperidin and 18kg mass fraction of 10% sodium hydroxide solution into the reactor, stirring and dissolving, then adding 0.0625kg catalyst palladium carbon, sealing the reactor, replacing the air in the reactor with nitrogen, Then feed hydrogen to replace nitrogen at normal temperature, stir and react under normal pressure for 12 hours, after the reaction is completed, use nitrogen to replace hydrogen in the reactor, then stop the reaction, and extract the reaction solution;

[0038] Step 2. Adjust the pH of the reaction solution to 6, crystallize at room temperature for 12 hours, and filter to obtain crystal A; the obtained filtrate is adsorbed with macroporous resin D101, and after adsorption, it is eluted with purified water to remove the salt in the filtrate; then, use 18 The volume fraction of twice the column volume is eluted with 20% ethanol, an...

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Abstract

The invention discloses a preparation method of neohesperidin dihydrochalcone. The preparation method comprises 1, adding neohesperidin and an alkaline solution into a reactor, carrying out stirring dissolution, adding a palladium-carbon catalyst into the reactor, enclosing the reactor, replacing air in the reactor with nitrogen gas, feeding hydrogen into the reactor at the normal temperature to replace nitrogen gas, carrying out a stirring reaction process under normal pressure, after the reaction is finished, replacing the hydrogen gas in the reactor with nitrogen gas, stopping the reaction and pumping out the reaction solution, and 2, adjusting pH of the reaction solution to 5-6, carrying out crystallization at the normal temperature, carrying out filtration to obtain crystals A, adsorbing the filtrate through a macroporous resin, then carrying out elution through purified water to remove the salt in the filtrate, carrying out elution through ethanol, collecting the eluate, carrying out condensation and crystallization, carrying out filtration to obtain crystals B, merging the crystals A and B, and carrying out freeze drying to obtain neohesperidin dihydrochalcone. The preparation method realizes synthesis of neohesperidin dihydrochalcone at the normal temperature under normal pressure through one kettle way, has simple processes and realizes a low production cost and high product neohesperidin dihydrochalcone purity.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of neohesperidin dihydrochalcone. Background technique [0002] Neohesperidin dihydrochalcone is a flavonoid derivative extracted from natural citrus plants and hydrogenated. It has the characteristics of high sweetness, refreshing taste, long-lasting aftertaste, low calorie, non-toxic, and good stability. , the sweetness is about 1400-1800 times of sucrose. It has the characteristics of excellent taste improvement and long duration of sweetness. It is mainly used as sweetener and taste-screening agent for the improvement, enhancement and overall Improvement, has an excellent effect of shielding bitterness, when used alone as an artificial sweetener, its concentration is 15-20mg / L; it has a unique effect of enhancing taste, as a synergist, only need to add 4 -5mg / L neohesperidin dihydrochalcone just showed good flavor synergism; as a p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/00C07H1/06
CPCC07H1/00C07H1/06C07H15/203
Inventor 竹文坤杨小艳袁小红罗勇
Owner SUZHOU YOUDAN INTERNET TECH CO LTD
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