Method for preparing L-ascorbic acid-2-phosphate ester and salt

A technology of ascorbate and ascorbic acid, which is applied in the field of preparation of vitamin C derivatives, can solve the problems of loss of esterification activity, easy moisture absorption, stickiness, decomposition and destruction, etc., and achieve the effect of high L-ascorbic acid content

Inactive Publication Date: 2006-04-19
HEBEI WELCOME PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0027] As a result, when phosphorus pentoxide is directly added alone, phosphorus pentoxide is very easy to absorb moisture and become sticky, decomposes and destroys, and when it is added to a reaction system with water as the medium, it directly reacts violently with water and loses the esterification activity.

Method used

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  • Method for preparing L-ascorbic acid-2-phosphate ester and salt
  • Method for preparing L-ascorbic acid-2-phosphate ester and salt
  • Method for preparing L-ascorbic acid-2-phosphate ester and salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Preparation of L-ascorbic acid-2-monophosphate monosodium monocalcium salt

[0077]

[0078] Into a 250 ml flask equipped with a stirrer, a thermometer, an air duct, a pH meter electrode, and a dropping funnel, a nitrogen stream was introduced, 15 ml of water and 17.6 g (100 mmol) of L-ascorbic acid were added, stirred to dissolve, and the solution was cooled to below 0°C. While stirring, 10 ml (100 mmol) of a 10 mol / L sodium hydroxide solution was added dropwise. Control the temperature at -5°C±3°C, add a mixture of 7.81 g (55 mmol) of phosphorus pentoxide and 8.15 g (110 mmol) of calcium hydroxide in portions, the molar ratio of L-ascorbic acid to phosphorus pentoxide is : 1:0.55, the molar ratio of phosphorus pentoxide to calcium hydroxide is 1:2. It takes about 2 to 3 hours to finish adding. Maintain -5~0°C for 2 hours, and 0~30°C for 4 hours. Concentrated sulfuric acid was added dropwise until the pH of the reactant was 9, 85 ml of 95% ethanol was added, sti...

Embodiment 2

[0081] Preparation of L-ascorbic acid-2-monophosphate disodium hemicalcium salt

[0082]

[0083] The reaction conditions are as example 1

[0084] Add 10 ml of water to 17.6 g (100 mmol) of L-ascorbic acid, stir to dissolve, and cool the solution to below 0°C. Add 10 milliliters (100 millimoles) of 10 mol / liter sodium hydroxide solution dropwise, add the mixture of 7.81 grams (55 millimoles) of phosphorus pentoxide and 4.08 grams (55 millimoles) of calcium hydroxide in stages, L- The molar ratio of ascorbic acid to phosphorus pentoxide is 1:0.55, and the molar ratio of phosphorus pentoxide to calcium hydroxide is 1:1. During the reaction, 10 mol / L sodium hydroxide solution was added dropwise to maintain pH 10-12. After the reaction, adjust the pH to 8.5-9 with sulfuric acid, add 80 ml of water to dilute, and then spray dry to obtain a light yellow powder product.

[0085]HPLC analysis measures, the L-ascorbic acid of 38.4% is L-ascorbic acid-2-monophosphate di-sodium he...

Embodiment 3

[0087] Preparation of L-ascorbic acid-2-monophosphate calcium salt

[0088]

[0089] The reaction conditions are as example 1

[0090] 17.6 g (100 mmol) of L-ascorbic acid was added to 20 ml of water, stirred and dissolved, and the solution was cooled to below 0°C. Add dropwise 18.5 grams (50 millimoles) of 20% (W / W) calcium hydroxide suspension, add 7.10 grams (50 millimoles) of phosphorus pentoxide and 7.41 grams (100 millimoles) of calcium hydroxide in portions to prepare The mixture, the molar ratio of L-ascorbic acid to phosphorus pentoxide is 1:0.5, and the molar ratio of phosphorus pentoxide to calcium hydroxide is 1:2. After the reaction, adjust the pH to 9 with sodium hydroxide solution and sulfuric acid, add 100 ml of 95% ethanol, stir for 0.5 hour, filter, and dry to obtain a white powdery product.

[0091] HPLC analysis measures, the L-ascorbic acid of 36.2% is L-ascorbic acid-2-monophosphate calcium salt in the product, the L-ascorbic acid (L-ascorbic acid-2-...

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Abstract

A process for preparing L-ascorbate-2-phosphate and its salts, including L-ascorbate-2-monophosphate, L-ascorbate-2-polyphosphate and their salts, features the esterifying reaction between L-ascorbate and phosphuric acid esterifying agent in water. Said phosphoric acid esterifying agent is the mixture of P2O5 and the hydroxide or oxide of alkali-earth metal or hydroxide of alkali metal.

Description

Technical field: [0001] The invention belongs to the field of preparation of vitamin C derivatives, more precisely, belongs to L-ascorbic acid-2-phosphate and its salt (Vc-2-phosphate salt), including L-ascorbic acid-2-monophosphate and L-ascorbic acid-2-phosphate - Process for the preparation of ascorbic acid-2-polyphosphate and salts thereof. Background technique: [0002] L-Ascorbic acid (also known as vitamin C, Vc) is an important substance necessary for living organisms. It is widely used in medicine, food and beverage, health and beauty, animal breeding, feed, fresh-keeping, chemical and other fields. Since L-ascorbic acid has strong reducing properties, it is easily oxidized and damaged during its manufacture, processing, storage and use, which limits its use in certain areas. [0003] L-ascorbic acid-2-phosphate (also known as vitamin C-2-phosphate, Vc-2-phosphate) is a highly stable L-ascorbic acid derivative that has appeared in the international market in recen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/572
Inventor 邢振堂封玉彬王芳张建成郭栋
Owner HEBEI WELCOME PHARMACEUTICAL CO LTD
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