Method for preparing D-calcium pantothenate

A technology of calcium pantothenate and hydrochloric acid, applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems affecting the industrial production of calcium D-pantothenate, low yield of calcium D-pantothenate, etc. The effect of water generation, high yield and simple process

Active Publication Date: 2011-01-19
XINFA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

At present, domestic and foreign manufacturers mostly use calcium oxide or calcium hydroxide as a calcifier, which has the advantage of low cost, but water is generated during the reaction process, and the acylation process has strict water requirements, resulting in a low yield of D-calcium pantothenate , generally only about 80%, affecting the industrialized production of D-calcium pantothenate

Method used

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  • Method for preparing D-calcium pantothenate
  • Method for preparing D-calcium pantothenate

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preparation example Construction

[0042] Since regulating moisture can promote the crystallization of calcium pantothenate, the preparation method of the present invention also includes the step of adding deionized water to regulate moisture after the acylation reaction. Among them, it is preferable to add deionized water to adjust the water content to 3.7-4.2%.

[0043] The method for preparing D-calcium pantothenate in the present invention does not use calcium oxide or calcium hydroxide as a calcifying agent, which can avoid the generation of water in the reaction process, so that the acylation process can be carried out better. On the other hand, the method for preparing D-calcium pantothenate of the present invention has a simple process, only needs to add 732 type calcium ion exchange resin, and the 732 type calcium ion exchange resin can be recycled and regenerated, without the generation of three wastes, which is a clean process. In addition, the yield of D-calcium pantothenate prepared by this method ...

Embodiment 1

[0046] Heat 165 grams of 30% sodium hydroxide solution to 90°C, control the temperature at 90±3°C, add dropwise 80 grams of 98% 3-aminopropionitrile, and drop it in 3 hours. Incubate at 2°C for 1 hour, evaporate under reduced pressure for half an hour to drive off the ammonia in the reaction liquid, drop the temperature to 50°C and add concentrated hydrochloric acid to adjust the pH=8.5, filter to remove a small amount of insoluble impurities, concentrate the filtrate under reduced pressure, and then cool down to crystallize to obtain 3-amino A mixture of sodium propionate and sodium chloride. After drying the mixture, add 1600 grams of methanol to dissolve, filter and discharge salt, add 400 grams of 732 type calcium ion exchange resin to the filtrate, control the temperature at 30°C and stir for 3 hours. Recover the resin by filtration, cool the filtrate to 10°C, add 152 grams of D-pantolactone, control the temperature at 10°C, keep stirring and react for 4 hours, add 2 gram...

Embodiment 2

[0048] Heat 209 grams of 30% sodium hydroxide solution to 90°C, control the temperature at 90±3°C, add dropwise 80 grams of 98% 3-aminopropionitrile, drop it in 3 hours, after the addition is complete, raise the temperature to 96°C and control the temperature at 98±3°C Incubate at 2°C for 1 hour, evaporate under reduced pressure for half an hour to drive off the ammonia in the reaction solution, adjust the pH to 9.5 with hydrochloric acid, filter to remove a small amount of insoluble impurities, concentrate the filtrate under reduced pressure, and then cool down to crystallize to obtain sodium 3-aminopropionate and sodium chloride mixture. After drying the mixture, add 2000 grams of methanol to dissolve, filter and discharge salt, add 450 grams of 732 type calcium ion exchange resin to the filtrate, control the temperature at 20°C and stir for 8 hours. Recover the resin by filtration, cool the filtrate to 10°C, add 146 grams of D-pantolactone, control the temperature at 0°C, k...

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Abstract

The invention relates to the field of chemical synthesis and discloses a method for preparing D-calcium pantothenate. The method comprises the following steps of: reacting 3-aminopropionitrile with aqueous solution of sodium hydroxide or potassium hydroxide at the temperature of between 96 and 100 DEG C, adding hydrochloric acid to regulate the pH value, and concentrating and crystallizing; dissolving the prepared crystal by using methanol, and filtering to remove salt; and performing ion exchange with 732-type calcium ion exchange resin, carrying out acylation reaction between reaction liquid and D-pantolactone, crystallizing at the temperature of between 15 DEG C below zero and 10 DEG C below zero, and drying to prepare the D-calcium pantothenate, wherein the molar ratio of the 3-aminopropionitrile to the sodium hydroxide and the potassium hydroxide is 1:1.1-1.4, and the molar ratio of the 3-aminopropionitrile to the D-pantolactone 1:1-1.1. The method for preparing the D-calcium pantothenate has the advantages of not using calcium oxide or calcium hydroxide as a calcification agent, avoiding water generation in the reaction process so as to ensure the smooth acylation process, along with simple process, high yield, recycled 732-type calcium ion exchange resin, no generation of three wastes, and contribution to industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing calcium D-pantothenate. Background technique [0002] Pantothenic acid, also known as pantothenic acid, also known as vitamin B5, is a water-soluble B vitamin. It is named pantothenic acid because it is widely found in animals and plants in nature. Pantothenic acid is a component of coenzyme A, which plays an important role in the metabolism of fat, protein and sugar in the body. It has the function of producing antibodies and also plays an important role in maintaining hair, skin and blood health. The main form of pantothenic acid is D-calcium pantothenate, which is widely used in food, medicine and feed additives. [0003] Pantothenic acid is widely found in food, but it will be lost in a large amount during processing. Therefore, D-calcium pantothenate is often added to food as a nutritional enhancer to promote human health and improve mental adaptabil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/12C07C231/02
Inventor 马成兵陈军王涛
Owner XINFA PHARMA
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