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Method for synthesizing magnesium ascorbyl phosphate

A technology of magnesium phosphate and vitamin, applied in the field of preparation of vitamin C derivatives, can solve the problems of irritation to mucous membranes, necrotic vision, irritation and corrosiveness, etc., and achieves the effect of improving yield and simplifying steps

Active Publication Date: 2018-07-17
安徽泰格生物技术股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, most industries use the group protection method to synthesize magnesium vitamin C phosphate, and use phosphorus oxychloride as a phosphorylation reagent, but phosphorus oxychloride is relatively toxic, and the volatilized gas is toxic, irritating and corrosive. It can irritate the mucous membrane and cause eye pain, and if it splashes into the conjunctival sac, it will cause necrosis and complete loss of vision, and the use of phosphorus oxychloride will also bring in more chloride ions, which will bring great pressure to subsequent processing and purification. Therefore, it is necessary to find a clean and safe phosphorylation reagent to replace phosphorus oxychloride and become the direction of synthetic vitamin C phosphate magnesium

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  • Method for synthesizing magnesium ascorbyl phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Add 85ml of acetone and 1ml of acetyl chloride into a dry 500ml four-necked flask equipped with mechanical stirring, a thermometer and a drying tube, and add 13.5g of vitamin C while stirring. The reaction temperature is 25°C and stirred for 3 hours.

[0032] 2. Weigh 4.3g of potassium hydroxide and dissolve it in 130ml of water. Slowly add it into the above-mentioned reacted feed solution under stirring. Evaporate acetone under reduced pressure, add water to 135ml, then add 37.1ml of pyridine, and cool to 0-2°C , use 10mol / L potassium hydroxide to adjust the pH of the reaction solution at 12-12.5, while adding dropwise a saturated aqueous solution of potassium pyrophosphate (25°C, 27g potassium pyrophosphate+15ml water), while keeping the reaction temperature at 0-2°C, the reaction solution The pH is 12-12.5, and the reaction is continued for 30 minutes after the dropwise addition is completed in 2 hours.

[0033] 3. After recovering pyridine under reduced pressure,...

Embodiment 2

[0035] Embodiment 2 is basically the same as Embodiment 1, and its difference is:

[0036] In the step (1), the reaction time was 2 hours, and the acetyl chloride consumption was 0.6ml;

[0037] In step (2), the reaction temperature is controlled at 2-5°C; the total reaction time is controlled at 1.5 hours;

[0038] In step (3), the reaction temperature is controlled at 40°C, and the reaction time is controlled at 1 hour;

[0039] 17.5 g of the finished product of vitamin C phosphate magnesium was obtained, with a yield of 60.1% and a content of 95.1% (determined by high-pressure liquid phase method).

Embodiment 3

[0041] Embodiment 3 is basically the same as Embodiment 1, and its difference is:

[0042] In the step (1), the reaction time is 4 hours, and the acetyl chloride consumption is 1.2ml;

[0043] In step (2), the reaction temperature is controlled at -2-0°C; the total reaction time is controlled at 3.5 hours;

[0044] In step (3), the reaction temperature is controlled at 30°C, and the reaction time is controlled at 1.5 hours;

[0045] 19.5 g of vitamin C magnesium phosphate finished product was obtained, the yield was 67.0%, and the content was 97.5% (determined by high-pressure liquid phase method).

[0046] It can be seen from the above examples that the method of the present invention can obtain magnesium vitamin C phosphate products that meet GB1903.24-2016 without using highly polluting and highly toxic phosphorus oxychloride, which simplifies the product purification steps and has a higher yield .

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Abstract

The invention provides a method for synthesizing magnesium ascorbyl phosphate. The method comprises the following steps: (1) reacting vitamin C with acetone by using acetyl chloride as a catalyst; (2)adding a potassium hydroxide solution into the reaction solution obtained in the step (1), separating and recovering the acetone, and performing a reaction with potassium hydroxide and potassium pyrophosphate in a pyridine aqueous solution system; and (3) separating and recovering pyridine in the liquid obtained after the reaction in the step (2), treating the obtained liquid by using cation exchange resin, and performing a reaction with magnesium oxide. The method provided by the invention adopts the potassium pyrophosphate as a phosphorylating reagent to replace phosphorus oxychloride, thepotassium pyrophosphate has almost no toxicity, and after the phosphorus oxychloride is replaced, a large number of anions such as chloride ions can be avoided from being introduced, so that post-treatment steps are reduced, product quality is improved, and the obtained product does not need to be recrystallized to meet national standard GB1903.24-2016.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a preparation method of vitamin C derivatives. Background technique [0002] The molecular formula and molecular weight of vitamin C magnesium phosphate are: C 12 h 12 o 18 P 2 Mg 3 10H 2 O=759.22 (according to the international relative atomic mass published in 2007). Its structural formula is [0003] [0004] Magnesium vitamin C phosphate, as a derivative of vitamin C, not only has all the functions of vitamin C, but also overcomes the shortcomings of vitamin C that are sensitive to light, heat, metal ions, etc., and are easily oxidized. As a nutritional additive, it can be widely used in various fortified foods, nutritional health products and beverages. Magnesium Vitamin C Phosphate is stable in nature, has excellent anti-oxidation and quality preservation, and can effectively prolong the storage period of food. It can be used as a color-preserving and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/655
Inventor 王珂
Owner 安徽泰格生物技术股份有限公司