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The preparation method of d-panthenol triacetate

A technology of panthenol triacetate and panthenol, which is applied to the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of harsh conditions for removing acetic acid, complicated steps, and harsh process conditions, and achieve The preparation method is simple and easy, the quality is excellent, and the effect of reducing the temperature and vacuum degree requirements for acetic acid removal

Active Publication Date: 2018-11-13
重庆鑫富化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese patent CN201610135191D has harsh conditions for removing acetic acid and complex washing process
If 4-dimethylaminopyridine is insoluble in water, catalyst residues are not easy to remove during extraction and washing
In summary, the synthesis method of D-panthenol triacetate generally has the problems of complex steps, harsh process conditions, difficulty in large-scale production and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 205.3g (1mol) of D-panthenol and 1.53g of p-toluenesulfonic acid into a 1000mL three-neck flask, slowly add 408.4g (4.0mol) of acetic anhydride and stir evenly, the reaction is exothermic, and the reaction temperature should not exceed 85°C. After the addition of acetic anhydride, the reaction solution was kept at 80° C. for 8 hours. While reacting, acetic acid was distilled off under reduced pressure, and the absolute pressure was 14kPa. After the reaction is completed, the reaction solution is obtained.

[0029] Water was added to the reaction solution four times, 50 g of water was added each time, the temperature was raised to 70° C., and the absolute pressure was 3.5 kPa for vacuum distillation for 1 hour. Acetic acid and water were distilled off to obtain a concentrate.

[0030] Add 500 mL of ethyl acetate and 150 mL of water to the concentrate, mix well, and adjust the pH to 7.5 with 10% aqueous sodium carbonate.

[0031] The extraction was allowed to sta...

Embodiment 2

[0038] Weigh 205.3g (1mol) of D-panthenol and 3.5g of p-toluenesulfonic acid into a 1000mL three-necked flask, slowly add 490.g (4.8mol) of acetic anhydride and stir evenly, the reaction is exothermic, and the reaction temperature should not exceed 85°C . After the addition of acetic anhydride, the reaction solution was kept at 75° C. for 9 hours. While reacting, acetic acid was distilled off under reduced pressure, and the absolute pressure was 9kPa. After the reaction is completed, the reaction solution is obtained.

[0039] Water was added to the reaction solution four times, adding 50 g of water each time. The temperature was raised to 70° C., and the absolute pressure was 3.5 kPa for vacuum distillation for 1 hour. Acetic acid and water were distilled off to obtain a concentrate.

[0040] Add 500 mL of ethyl acetate and 150 mL of water to the concentrate, mix well, and adjust the pH to 7.5 with 10% aqueous sodium carbonate.

[0041] The extraction was allowed to stan...

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Abstract

The invention belongs to the technical field of preparation of chemicals and particularly relates to a preparation method of D-panthenyl triacetate. The preparation method comprises the following steps: adding a p-toluene sulfonic acid catalyst into D-panthenol; slowly adding acetic anhydride and mixing and stirring; carrying out reduced pressure distillation to remove acetic acid; controlling a reaction temperature to be 65 DEG C-85 DEG C and the reaction time to be 6h to 12h, wherein the mol adding ratio of the D-panthenol to the acetic anhydride is 1 to (3.3 to 6.0) and the dosage of the p-toluene sulfonic acid catalyst is 0.5% of the total weight of the added D-panthenol and acetic anhydride; and then, removing the acetic acid through steam stripping, extracting, washing with water, carrying out reduced pressure distillationto obtain a product. According to the method provided by the invention, the p-toluene sulfonic acid is used as the catalyst and is used for removing the acetic acid under the decompression condition through reaction, so that the dosage of the catalyst is extremely reduced, the quality of the obtained product is high, and the yield reaches 90%.

Description

technical field [0001] The invention belongs to the technical field of chemical preparation, and in particular relates to a preparation method of D-panthenol triacetate. Background technique [0002] D-panthenol triacetate is a pantothenic acid series product, which includes panthenol, calcium pantothenate, panthenol ethyl ether, pantethine, etc. D-panthenol triacetate, like D-ubithenol, is converted into coenzyme A after entering the human body to function. D-panthenol triacetate is mainly used in cosmetic products according to its product characteristics, such as sunscreen skin care products, shampoo and conditioner, anti-aging skin care products. As an ingredient of cosmetics, D-panthenol triacetate mainly has the functions of anti-protein oxidation, alleviating skin redness, improving oily skin, reducing melanin precipitation, and brightening the skin. [0003] The artificial synthesis of D-panthenol triacetate is attracting more and more attention. Among them, US20050...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/12C07C231/24C07C235/08
CPCC07C231/12C07C231/24C07C235/08
Inventor 姜伟林杨可武黄晓余建新白彦兵
Owner 重庆鑫富化工有限公司
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