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Preparation method of calcium gluconate

A technology of calcium gluconate and glucose, which is applied in the field of medicine, can solve the problems of high cost, constant synthesis yield, and long cycle, and achieve the effects of short preparation process steps, high reaction selectivity, and easy-to-obtain raw materials

Active Publication Date: 2019-09-20
YANGZHOU ZHONGBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production methods of calcium gluconate raw materials mainly include electrolytic oxidation, catalytic oxidation and fermentation. At present, most domestic manufacturers adopt the fermentation method, but there are still problems such as cultivation, separation and by-products of the black U.S. military are not easy to control; electrolysis The oxidation method has disadvantages such as large investment, high cost, high energy consumption, and long cycle; catalytic oxidation is a relatively new chemical synthesis method at present, but the catalytic oxidation method requires expensive precious metal reagents, and the cost is not easy to control
[0004] In addition, the laboratory generally uses hydrogen peroxide or bromine water to oxidize glucose into gluconic acid, and calcium gluconate can be obtained after adding calcium carbonate for neutralization, but the synthesis yield of this method remains unchanged and low

Method used

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  • Preparation method of calcium gluconate
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  • Preparation method of calcium gluconate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 5kg glucose and 5L water into a 20L reaction vessel, add about 43.4g Tempo and 77.2g phase transfer catalyst tetrabutylammonium chloride, slowly stir and drop an aqueous solution of 1.5 times the mole amount of sodium hypochlorite at room temperature, and dropwise add 1.03kg of calcium hydroxide aqueous solution, stirred at room temperature for 1h, then concentrated under reduced pressure to 1 / 2 of the original volume, finally added an equal volume of ethanol, stirred, crystallized, filtered to obtain calcium gluconate, dried under reduced pressure to obtain 5.319kg, collected The yield is 85.5%, and the purity is 99.6%.

[0029] The IRAffinity-1S WL infrared tester of SHIMADZU was used to measure the infrared spectrum of the product, and the results are shown in figure 1 , verify that the product is calcium gluconate.

Embodiment 2

[0031] Add 5kg of glucose and 10L of water into a 20L reaction vessel, add about 43.4g of Tempo and 77.2g of phase transfer catalyst tetrabutylammonium chloride, slowly stir and drop an aqueous solution of 1.2 times the mole amount of sodium hypochlorite at room temperature, and dropwise add 1.03kg of calcium hydroxide aqueous solution, stirred at room temperature for 1h, then concentrated under reduced pressure to 1 / 2 of the original volume, finally added an equal volume of ethanol, stirred, crystallized, filtered to obtain calcium gluconate, dried under reduced pressure to obtain 5.114kg, and collected The yield is 82.2%, and the purity is 99.5%.

[0032] figure 2 For the infrared spectrum of the calcium gluconate prepared in Example 2, it is verified that the product is calcium gluconate.

Embodiment 3

[0034] Add 5kg of glucose and 15L of water into a 20L reaction vessel, add about 86.8g of Tempo and 77.2g of phase transfer catalyst tetrabutylammonium chloride, slowly stir and drop an aqueous solution of 1.2 times the mole amount of sodium hypochlorite at room temperature, and dropwise add 1.03 kg of calcium hydroxide aqueous solution, stirred at room temperature for 1 h, then concentrated under reduced pressure to 1 / 3 of the original volume, finally added an equal volume of ethanol, stirred, crystallized, filtered to obtain calcium gluconate, dried under reduced pressure to obtain 5.002 kg, and collected The yield is 80.9%, and the purity is 99.4%.

[0035] image 3 For the infrared spectrum of the calcium gluconate prepared in Example 3, it is verified that the product is calcium gluconate.

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Abstract

The invention discloses a preparation method of calcium gluconate. The preparation method comprises following steps: adding a catalytic amount of Tempo and a phase transfer catalyst into a water solution of glucose; stirring the solution at a room temperature, dropwise adding a water solution of sodium hypochlorite at the same time, carrying out reactions for 4 to 5 hours, then adding a water solution of calcium salts, keeping on stirring the solution at a room temperature for 1 to 2 hours, then performing vacuum concentration, adding the reaction product into an organic solvent, stirring the organic solvent, carrying out crystallization, and filtering. According to the preparation method, a Tempo-NaClO system is used to oxidize glucose in the presence of a phase transfer catalyst, and then oxidized glucose and calcium hydroxide carry out slat forming reactions to generate calcium gluconate. Compared with the prior art, the preparation technology has short steps, the raw materials are easily available and cheap, the reaction selectivity is high, the yield is high, and the post treatment is simple. The calcium gluconate yield of the preparation technology can reach 85% or more, and the purity can reach 99% or more.

Description

technical field [0001] The invention relates to a new method for preparing calcium gluconate (Calcium (2R, 3S, 4R, 5R)-2, 3, 4, 5, 6-pentahydroxyhexanoate), which belongs to the technical field of medicine. Background technique [0002] Calcium gluconate is a medicine and fine chemical. As a drug, it can promote the calcification of bones and teeth and maintain the normal excitability of muscles and muscles; it is mainly used in the treatment of calcium deficiency, acute hypocalcemia, alkalosis and tetany and allergy caused by hypoparathyroidism. Sexual diseases, rescue of magnesium and fluorosis, and application of cardiac resuscitation. [0003] At present, the production methods of calcium gluconate raw materials mainly include electrolytic oxidation, catalytic oxidation and fermentation. At present, most domestic manufacturers adopt the fermentation method, but there are still problems such as cultivation, separation and by-products of the black U.S. military are not ea...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C59/105
CPCC07C51/412C07C59/105
Inventor 朱克明金昌明吕建东
Owner YANGZHOU ZHONGBAO PHARMA
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