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A kind of preparation method of l-ascorbyl palmitate

A technology of ascorbyl palmitate and ascorbic acid, applied in the field of preparation of L-ascorbyl palmitate, can solve problems such as destruction of materials, unsuitable application, system temperature rise, etc., and achieves improved safety, short filtration time, and large solid particles. Effect

Active Publication Date: 2019-04-26
SHENZHEN HAIBIN PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is also found through experiments that adding the ice-water mixture to the reaction solution after the esterification reaction will still cause a sharp increase in the temperature of the system; and it is easy to emulsify when extracted with ethyl acetate
In addition, both toluene and methylene chloride are toxic and are not suitable for applications in food and other fields; and vacuum distillation of the organic phase will destroy materials and affect product quality
[0006] Therefore, although the sulfuric acid catalyzed direct esterification method is relatively mature, there are still deficiencies in the post-treatment of the esterification reaction in the prior art, and further improvement is needed to improve production safety and product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1) Add 10kg of concentrated sulfuric acid to a dry and clean four-neck flask, cool down to 20-25°C, then add 1kg of L-ascorbic acid and stir for 20min to dissolve; ℃.

[0049] 2) After the reaction is complete, cool the system down to 0-5°C, add 9.8kg of ethyl acetate dropwise, and control the system temperature at 25-35°C; after the dropwise addition, the temperature drops to about 25°C, and slowly add 21.8kg of ice water, The temperature is controlled at 35-45°C. When the temperature does not rise significantly, quickly add the remaining ice water dropwise.

[0050] 3) After adding the ice water dropwise, quickly filter (taking 30min), wash the filter cake and the reaction vessel with 1.0kg of ethyl acetate, add the filter cake to 4.9kg of ethyl acetate, heat and stir to dissolve, and control the temperature at 45-50 ℃; after the dissolution is complete, add 6kg of water, raise the temperature to 45-50℃, stir for 30min, let stand for 15min, separate layers, discard t...

Embodiment 2

[0053] 1) Add 8kg of concentrated sulfuric acid to a dry and clean four-neck flask, cool down to 20-25°C, then add 1kg of L-ascorbic acid and stir for 20 minutes to dissolve; after dissolving, add 0.8kg of palmitic acid and stir for 24 hours to control the temperature at 25-27°C .

[0054] 2) After the reaction is complete, cool the system down to 0-5°C, add 8kg of ethyl acetate dropwise, and control the system temperature at 25-35°C; 35-45°C, when the temperature does not rise significantly, quickly add the remaining ice water dropwise.

[0055] 3) After adding ice water dropwise, quickly filter (taking 25min), wash the filter cake and the reaction vessel with 1.0kg of ethyl acetate, add the filter cake to 4kg of ethyl acetate, heat and stir to dissolve, and control the temperature at 45-50°C After the dissolution is complete, add 5kg of water, raise the temperature to 45-50°C, stir for 30min, let it stand for 15min, separate layers, discard the lower aqueous phase; add 2kg ...

Embodiment 3

[0058] 1) Add 5kg of concentrated sulfuric acid to a dry and clean four-neck flask, cool down to 20-25°C, then add 1kg of L-ascorbic acid and stir for 20 minutes to dissolve; after dissolving, add 1kg of palmitic acid and stir for 24 hours, controlling the temperature at 20-22°C.

[0059] 2) After the reaction is complete, lower the temperature to 0-5°C, add 5kg of ethyl acetate dropwise, and control the temperature of the system at 25-35°C; ~45°C; when the temperature does not rise significantly, quickly add the remaining ice water dropwise.

[0060] 3) After adding the ice water dropwise, quickly filter (taking 28min), wash the filter cake and the reaction vessel with 1.0kg of ethyl acetate, add the filter cake to 6kg of ethyl acetate, heat and stir to dissolve, and control the temperature at 45-50°C After the dissolution is complete, add 7kg of water, raise the temperature to 45-50°C, stir for 30min, let stand for 15min, separate layers, discard the lower aqueous phase; add...

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PUM

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Abstract

The invention provides a preparation method for L-ascorbic acid palmitate. The preparation method comprises the following steps: carrying out esterification reaction on L-ascorbic acid and palmitic acid under concentrated sulfuric acid catalysis, firstly dropwise adding ethyl acetate into a reaction system after reaction is complete, dropwise adding ice water, and filtering to obtain an L-ascorbic acid palmitate crude product; through ethyl acetate recrystallization, obtaining a target product L-ascorbic acid palmitate. The preparation method has the advantages of safe and controllable technology, simplified aftertreatment procedure and high product purity, conforms to a standard stipulated by the European Pharmacopoeia, and is more suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a preparation method of L-ascorbyl palmitate. Background technique [0002] L-ascorbyl palmitate (L-AP for short), also known as vitamin C palmitate, is a new type of multifunctional antioxidant, which has been evaluated by the Food Additives Committee of the World Health Organization as nutritious, It is a non-toxic, efficient and safe food additive, and it has been recorded in the British and American Pharmacopoeia, and has been widely used in food, medicine, cosmetics and other fields. [0003] At present, the production process routes of L-ascorbyl palmitate mainly include acid chloride method, direct esterification method, transesterification method and lipase method. The acid chloride method requires harsh reaction conditions and special reactors, and is not suitable for industrial production. The lipase method is immature and is still under discussion. [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/62
CPCC07D307/62
Inventor 罗文军胡金军任鹏
Owner SHENZHEN HAIBIN PHARMA
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