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Industrial preparation method of high-purity sodium pantothenate

A high-purity sodium pantothenate technology, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as time-consuming, unsuitable for industrial production, and failure to achieve crystallization and impurity removal. Quality and yield, suitable for industrial production, and the effect of avoiding difficult dissolution

Active Publication Date: 2015-05-06
HEBEI YIPIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Repeated heating consumes a lot of heat, heat loss is large, time-consuming and labor-intensive; and in the whole synthesis process, there is no effective purification method, and the product is evaporated to dryness so that impurities (new impurities and unreacted raw materials) remain in the crude product to the maximum extent. result in low product purity
[0011] Third, the crude product is recrystallized with absolute ethanol, and the total yield is only 44%
It is difficult to dissolve during recrystallization, easy to produce oil, time-consuming, waste of manpower, material and financial resources, and low yield. In addition, raw materials such as calcium pantothenate and sodium carbonate remain in the crude product, and the two are slightly soluble in ethanol, so recrystallization with ethanol cannot Effective removal, the purpose of crystallization and impurity removal is not achieved, the product quality cannot be guaranteed, and it is not suitable for industrial production

Method used

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  • Industrial preparation method of high-purity sodium pantothenate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 50 grams of calcium pantothenate into 150ml of purified water, stir to dissolve, add dropwise sodium carbonate solution (11.12 grams of sodium carbonate dissolved in 35ml of water), react for 20 minutes after the dropwise addition within 30 minutes, and then filter; add 0.5 grams of activated carbon to the filtrate , stirred for 30 minutes and then filtered through the membrane; when the membrane solution was concentrated under reduced pressure at 55°C to 75 grams of the remaining feed solution, 120 grams of absolute ethanol was added, and after stirring evenly, the feed solution was dropped into 600 grams of acetone, and then raised After crystallizing for 2 hours, filter and then vacuum-dry at 40-50°C to obtain 44 grams of sodium pantothenate dry product with a purity of 99.8%.

Embodiment 2

[0027] Add 50 grams of calcium pantothenate to 200ml of purified water, stir to dissolve, add dropwise sodium carbonate solution (11.12 grams of sodium carbonate dissolved in 35ml of water), react for 30 minutes after the dropwise addition within 30 minutes, and then filter; add 0.5 grams of activated carbon to the filtrate , stirred for 30 minutes and then filtered through the membrane; when the membrane solution was concentrated under reduced pressure at 55°C to 100 grams of the remaining feed solution, 200 grams of absolute ethanol was added, and after stirring evenly, the feed solution was dropped into 1000 grams of acetone, and then raised After crystallizing for 2 hours, filter and then vacuum-dry at 40-50°C to obtain 44.7 g of sodium pantothenate dry product with a purity of 99.7%.

Embodiment 3

[0029] Add 50 grams of calcium pantothenate to 250ml of purified water, stir to dissolve, add dropwise sodium carbonate solution (11.12 grams of sodium carbonate dissolved in 42ml of water), and react for 50 minutes after the dropwise addition within 30 minutes, then filter; add 0.5 grams of activated carbon to the filtrate , stirred for 30 minutes and then filtered through the membrane; when the membrane solution was concentrated under reduced pressure at 55°C to 115 grams of the remaining material liquid, 230 grams of absolute ethanol was added, and after stirring evenly, the material solution was dropped into 1700 grams of acetone to grow crystals Filter after 2 hours, and then vacuum-dry at 40-50°C to obtain 45 grams of sodium pantothenate dry product with a purity of 99.8%.

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Abstract

The invention discloses an industrial preparation method of high-purity sodium pantothenate. The method comprises the following steps: adding calcium pantothenate into purified water and dissolving to obtain calcium pantothenate solutions; adding sodium carbonate solutions into sodium pantothenate solutions, performing reaction, filtering and collecting filter liquid; adding active carbon into the filter liquid to be filtered and then filtered by a film; concentrating the liquid filtered by the film and adding ethanol; adding concentrated liquid into which ethanol is added into acetone; growing grains and drying to obtain sodium pantothenate. According to the industrial preparation method, high-temperature drying by distillation and multi-time repeated concentration are not needed, so that the working hours are shortened, and the side reaction is reduced; a special crystallizing condition is not needed, so that the problems that ethanol crystals are difficult to dissolve, easy in oil outflow and difficult to separate out are solved; because the process is simple, the working hours can be shortened by 1-2 times, and the production cost can be reduced by more than 50 percent. The used solvent is low in cost, the defects of high solubility of sodium pantothenate in ethanol and low yield are overcome, and the quality and the yield of the product are guaranteed; moreover, the purity of the product reaches 99.8 percent, and the yield is increased to 90 percent; therefore, the method is more suitable for industrial production.

Description

technical field [0001] The invention relates to an industrialized preparation method of water-soluble vitamin sodium pantothenate. Background technique [0002] Sodium pantothenate, English name D-Pantothenic Acid Sodium Salt, alias D-pantothenic acid sodium, chemical name (R)-N-(2,4-dihydroxy-3,3-dimethyl-1-oxobutyl)- Beta-alanine, monosodium salt, is the sodium salt form of pantothenic acid. Pantothenic acid, also known as pantothenic acid and vitamin B3, is a kind of vitamin B family. It can help cells form, maintain normal development and the development of the central nervous system, and maintain the normal function of the adrenal gland. It is indispensable when fat and sugar are converted into energy. It is also an essential substance for antibody synthesis and human body's utilization of aminobenzoic acid and choline. There are two forms of pantothenic acid, calcium salt and sodium salt, commonly used clinically. Calcium pantothenate and its tablets have been recor...

Claims

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Application Information

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IPC IPC(8): C07C235/12C07C231/24C07C231/12
Inventor 赵翠然贾宗英左凯亚王婷婷邱玉敏程瑶
Owner HEBEI YIPIN PHARMA
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