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Preparation method of vitamin A microcosmic salt

A technology of vitamins and phosphorus salts, applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of unstable phosphorus salt solution and difficult concentration, and achieve stable reaction, Raw materials are readily available and concentrated

Inactive Publication Date: 2013-09-11
广州巨元生化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The preparation method of vitamin A phosphorus salt is mentioned in U.S. Patent US4105855, adopts n-hexane extraction in the purification process of vitamin A phosphorus salt, removes some impurities in the phosphorus salt, but because water will be added in the extraction process, finally in Methanol is removed under vacuum in water. However, during the process of removing methanol, the phosphorus salt solution will generate a lot of foam, making it difficult to concentrate. At the same time, the phosphorus salt solution is unstable at high temperature.

Method used

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Examples

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Effect test

Embodiment 1

[0025] A method for preparing vitamin A phosphate salt, the specific steps are as follows:

[0026] Add 27.5 grams of triphenylphosphine to 120 grams of methanol. Under the protection of nitrogen, add 10 grams of concentrated sulfuric acid at 20°C, stir for 30 minutes, then cool to 10°C, and then add 63.6 grams of 1.5 million international units vitamin A acetate. Then the reaction was stirred at 25-30°C for 12 hours, concentrated under reduced pressure at 45°C to remove methanol, then 150g of acetone was added, refluxed for 30 minutes, then cooled to 5°C, stirred for 2 hours, filtered, and filtered with 50g of cold acetone The filter cake was washed twice and dried in vacuum at 50°C for 5 hours to obtain 47.5 grams of vitamin A phosphate salt, with a content of about 95% and a yield of 69.8%.

Embodiment 2

[0028] A method for preparing vitamin A phosphate salt, the specific steps are as follows:

[0029] Add 26.2 grams of triphenylphosphine to 100 grams of methanol, under the protection of nitrogen, add 9.9 grams of concentrated sulfuric acid at 20°C, stir for 30 minutes, then cool to 8°C, and then add 63.6 grams of 1.5 million international units vitamin A acetate. Then the reaction was stirred at 25-30°C for 12 hours, concentrated under reduced pressure at 40°C to remove methanol, then 100g of acetone was added, refluxed for 30 minutes, then cooled to 5°C, stirred for 2 hours, filtered, and 60g of cold acetone The filter cake was washed twice and dried in vacuum at 45°C for 5 hours to obtain 46.2 grams of vitamin A phosphate salt, with a content of about 94% and a yield of 67.9%.

Embodiment 3

[0031] A method for preparing vitamin A phosphate salt, the specific steps are as follows:

[0032] Add 28.8 grams of triphenylphosphine to 150 grams of methanol. Under the protection of nitrogen, add 12 grams of concentrated sulfuric acid at 20°C, stir for 30 minutes, then cool to 12°C, and then add 63.6 grams of 1.45 million IU vitamin A acetate. Then the reaction was stirred at 25-30°C for 16 hours, concentrated under reduced pressure at 45°C to remove methanol, then 150g of acetone was added, refluxed for 30 minutes, then cooled to 5°C, stirred for 2 hours, filtered, and filtered with 50g of cold acetone The filter cake was washed twice and dried in vacuum at 50°C for 5 hours to obtain 49.1 g of vitamin A phosphate salt with a content of about 96% and a yield of 72.2%.

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Abstract

The invention discloses a preparation method of vitamin A microcosmic salt. The method specifically comprises the following steps of: adding triphenylphosphine into an alcohol solvent, subsequently adding acid and vitamin A acetic ester, reacting for 6-24 hours at 15-60 DEG C, and crystallizing to obtain the vitamin A microcosmic salt. The preparation method of the vitamin A microcosmic salt adopts the crystallization mode, the concentration is easy to carry out, and the foam is prevented; and the method has the advantages that the process is simple to operate, the raw materials are available, the reaction is stable, the reaction condition is gentle, the cost is low, and the like. Besides, by utilizing the preparation method disclosed by the invention, the stability of the vitamin A microcosmic salt is improved, a high-content product is obtained, the yield of the product is greater than 65%, and the prepared vitamin A microcosmic salt can be directly used for preparing beta-carotene.

Description

[0001] Technical field [0002] The invention relates to the field of organic synthesis, in particular to a preparation method of vitamin A phosphate salt. [0003] Background technique [0004] β-carotene (C 40 H 56 ) Is one of the carotenoids and also an orange-yellow fat-soluble compound. It is the most ubiquitous and most stable natural pigment in nature. Many natural foods, such as green vegetables, sweet potatoes, carrots, spinach, papaya, mangoes, etc., are rich in β-carotene. Beta-carotene is an antioxidant with detoxification effect and an indispensable nutrient for maintaining human health. It has significant functions in anti-cancer, prevention of cardiovascular diseases, cataracts and antioxidants, and further prevents aging and senescence. A variety of degenerative diseases. Artificially synthesized β-carotene generally uses vitamin A as a raw material. In the process of synthesizing β-carotene, the synthesis of vitamin A phosphate is a very critical step. [0005] Th...

Claims

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Application Information

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IPC IPC(8): C07F9/54
Inventor 叶锦刘庆辉李建喜
Owner 广州巨元生化有限公司
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