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Preparation method of vitamin C palmitate

A palmitate and vitamin technology, applied in the direction of organic chemistry, can solve the problems of increased reaction yield, high recycling cost, and difficulty in product quality assurance, and achieve the effects of reducing impurities, improving product purity, and preventing oxidation

Inactive Publication Date: 2017-11-24
GUANGDONG GUANGYI TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But according to this patent scheme, in fact, the reaction yield is not significantly improved compared with the sulfuric acid method. Considering that polar aprotic solvents are generally relatively expensive water-soluble high-boiling substances, the recovery cost is relatively high, so the overall production of this method is relatively high. The cost is higher than that of the sulfuric acid method. In addition, there are more impurities produced by this patented method, and the product quality is difficult to guarantee, thus limiting the application of the acid chloride method in actual production.

Method used

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Examples

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Effect test

preparation example Construction

[0033] The preparation method of vitamin C palmitate of the present invention, it comprises the steps: provide L-ascorbic acid, dimethylacetamide and chloroform; Dimethylacetamide, chloroform and L-ascorbic acid are mixed, A mixed solution is formed; the mixed solution is dripped with a palmitoyl chloride solution under acidic conditions to carry out an esterification reaction; in the later stage of the esterification reaction, an inert gas, a reducing gas and / or a weak acid are introduced into the mixed solution gas until the end of the reaction. The invention introduces inert gas, reducing gas and / or weak acid gas into the esterification reaction system in the later stage of the esterification reaction to drive away excess hydrogen chloride produced by the esterification reaction, break the reaction balance, and promote the reaction to develop towards esterification; At the same time, adding the above-mentioned gas to cooperate with the reaction system can also prevent the o...

Embodiment 1

[0041] The preparation method of vitamin C palmitate described in the present embodiment comprises the steps of: adding 30ml dimethylacetamide at 0° C. Then add 8.8 grams of L-ascorbic acid and 15ml of chloroform or successively add 15ml of chloroform and 8.8 grams of L-ascorbic acid at 0°C, add anhydrous hydrogen chloride, stir to obtain a clear liquid, and put it at 0°C within 4 hours 27.5 grams of palmitoyl chloride was added dropwise. After the reactant was stirred at 0°C for 12h, nitrogen gas was introduced to continue the reaction for 6h, and then the temperature was raised to 20°C for 30min. After the reaction is over, add a dilution of 200ml of ethyl acetate and 200ml of water to the reaction system after gradually cooling down, stir at 0°C for 2 hours, and finally filter with suction at 0°C. The initial product, vitamin C palmitate, is vacuum-dried to obtain the finished product. Check the purity of the raw product. The finished product is 16.4 g (purity 99.8%), th...

Embodiment 2

[0043]The preparation method of vitamin C palmitate described in the present embodiment comprises the steps of: adding 30ml dimethylacetamide at 0° C. Then add 8.8 grams of L-ascorbic acid and 15ml of chloroform or successively add 15ml of chloroform and 8.8 grams of L-ascorbic acid at 0°C, add anhydrous hydrogen chloride, stir to obtain a clear liquid, and put it at 0°C within 4 hours 27.5 grams of palmitoyl chloride was added dropwise. After the reactant was stirred at 0° C. for 12 h, carbon dioxide gas was introduced to continue the reaction for 6 h, and then the temperature was raised to 20° C. for 30 minutes. After the reaction is over, add a dilution of 200ml of ethyl acetate and 200ml of water to the reaction material after gradually cooling down, stir at 0°C for 2 hours, and finally filter with suction at 0°C. The initial product, vitamin C palmitate, is vacuum-dried to obtain the finished product. Check the purity of the raw product. The finished product is 17.2 g ...

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Abstract

The invention discloses a preparation method of vitamin C palmitate. The method comprises steps as follows: L-ascorbic acid, dimethylacetamide and trichloromethane are provided; dimethylacetamide, trichloromethane and L-ascorbic acid are mixed to form a mixed solution; anhydrous hydrogen chloride is introduced into the mixed solution, a palmitoyl chloride solution is dropwise added for an esterification reaction; at the later stage of the esterification reaction, inert gas, reductive gas and / or weak acid gas is / are introduced into the mixed solution to remove surplus hydrogen chloride produced during a reaction until the reaction ends. Vitamin C palmitate prepared with the preparation method of high-quality vitamin C palmitate contains fewer impurities and is high in quality and higher in yield.

Description

technical field [0001] The invention relates to the technical field of preparation of VC esters, in particular to a preparation method of vitamin C palmitate. Background technique [0002] Vitamin C is also known as L-ascorbic acid, and palmitate is a long-chain fatty acid ester with 16 carbon atoms. Long-chain fatty acids and their derivatives have poor reactivity, and their esters can only be formed under relatively strong conditions. However, vitamin C has poor stability and is easily damaged by high temperature, acid-base or oxygen. It is necessary to obtain high-quality vitamin C with high yield Long chain fatty acid esters are very difficult. The sulfuric acid method is commonly used in production now. The raw material vitamin C is directly reacted with palmitic acid or methyl palmitate in a large amount of concentrated sulfuric acid. The concentrated sulfuric acid is used as a catalyst and solvent. After the reaction is completed, it is added to ice water for precipi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/62
CPCC07D307/62
Inventor 林洪
Owner GUANGDONG GUANGYI TECH IND
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