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Preparation method of L-ascorbyl palmitate

A technology of ascorbyl palmitate and ascorbic acid, which is applied in the field of preparation of L-ascorbyl palmitate, can solve the problems of low yield and poor purity of L-ascorbyl palmitate, achieves good appearance, improves quality and purity, and improves reagent quality. A wide range of effects

Inactive Publication Date: 2012-07-11
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the defects of low yield and poor purity of L-ascorbyl palmitate in the prior art, the purpose of this invention is to provide a kind of preparation method of L-ascorbyl palmitate

Method used

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  • Preparation method of L-ascorbyl palmitate
  • Preparation method of L-ascorbyl palmitate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation

[0025] Add 8.0g of L-ascorbic acid and 45.0ml of concentrated sulfuric acid into a 250.0mL three-necked flask, heat it to 30.0°C under stirring, slowly add 16.0g of palmitic acid dropwise, and keep the inner temperature of the three-necked flask at about 30.0°C during the dropping process. Minutes dropwise completed, constant temperature reaction 32h.

[0026] (2) Extraction

[0027] After the reaction, the reaction system was extracted with an ice-water mixture with a ratio of ice and water of 1:1. The volume of the ice-water mixture was about 180ml, and then the ice-water solution was extracted with ethyl acetate, and the extract was distilled under reduced pressure to obtain a solid , and dried in an oven at 50°C to obtain 17.1 g of a yellow solid crude product.

[0028] (3) refined

[0029] The resulting 17.1g solid and 68.0mL petroleum ether: absolute ethanol = 1:0.4 (volume ratio) were stirred in a three-necked flask at 55.0°C until the soluti...

Embodiment 2

[0031] (1) Preparation

[0032] Add 8.0g of L-ascorbic acid and 36.0ml of concentrated sulfuric acid to a 250.0mL three-necked flask, heat it to 27°C while stirring, slowly add 12.8g of palmitic acid dropwise, and keep the inner temperature of the three-necked flask at about 27°C during the dropping process for 20 minutes After the addition was completed, the reaction was carried out at a constant temperature for 30 hours.

[0033] (2) Extraction

[0034] After the reaction, the reaction system was extracted with an ice-water mixture with a ratio of ice and water of 1:1. The volume of the ice-water mixture was about 250ml, and then the ice-water solution was extracted with dichloromethane, and the extract was distilled under reduced pressure to obtain a solid , placed in a 50°C oven and dried to obtain 16.5 g of a yellow solid crude product.

[0035] (3) refined

[0036] The resulting 16.5g solid and 65.0mL petroleum ether: absolute ethanol = 1:0.45 (volume ratio) were stir...

Embodiment 3

[0038] (1) Preparation

[0039] Add 8.0g of L-ascorbic acid and 60.0ml of concentrated sulfuric acid into a 250.0mL three-necked flask, heat it to 30°C while stirring, slowly add 17.0g of palmitic acid, and keep the inner temperature of the three-necked flask at about 30°C during the dropping process for 40 minutes After the addition was completed, the reaction was carried out at a constant temperature for 35 hours.

[0040] (2) Extraction

[0041] After the reaction, the reaction system was extracted with an ice-water mixture with a ratio of ice and water of 1:1. The volume of the ice-water mixture was about 200ml, and then the ice-water solution was extracted with ethyl acetate, and the extract was distilled under reduced pressure to obtain a solid , placed in a 50°C oven and dried to obtain 18.2 g of a yellow solid crude product.

[0042] (3) refined

[0043] The resulting 18.2g solid and 70.0mL petroleum ether: absolute ethanol = 1:0.4 (volume ratio) were stirred in a t...

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Abstract

The invention relates to a preparation method of L-ascorbyl palmitate, which includes directly conducting esterification reaction on L- ascorbic acid and palmitic acid under the existence of concentrated sulfuric acid, adding an ice water mixture after reaction, conducting extraction through an organic solvent, conducting reduced pressure distillation on extraction liquid to obtain a coarse product, and conducting recrystallization on the coarse product through a mixed solvent of petroleum ether and ethanol to obtain the L-ascorbyl palmitate. The technical scheme of the preparation method improves quality and purity of the L-ascorbyl palmitate, and the product is good in appearance, stable in quality and capable of achieving national food grade standard. Further, the whole process is mild in reaction condition, convenient to operate and wide in reagent source. The preparation method of the food grade L-ascorbyl palmitate is ideal and effective.

Description

technical field [0001] The invention relates to the field of synthesis of fine chemicals, in particular to a preparation method of L-ascorbyl palmitate. Background technique [0002] With the rapid development of my country's food industry and the continuous improvement of people's living standards, more and more food has been put on the market, and the shelf life and quality of food have become the main issues that people care about. Therefore, various anti-corrosion and fresh-keeping measures must be taken to prolong the shelf life and shelf life of food and reduce the loss of nutrients. There are many specific methods, including canning, cold bulbing, drying, pickling, chemical preservation, and modern popular new technologies such as aseptic packaging, vacuum packaging, microwave sterilization, and radiation preservation. These methods each have their own characteristics and scope of application. . Among them, chemical antiseptic can effectively inhibit or kill the mic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/62
Inventor 孙建华詹永章李亚龙
Owner BENGBU BBCA MEDICINE SCI DEV
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