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Novel method for preparing medicinal despun hydroxyl methionine calcium

A technology of racemic calcium hydroxymethionine and liquid methionine, which is applied in the field of chemical synthesis of racemic calcium hydroxymethionine, can solve the problem of increasing operation steps and difficulty, not considering the existence of dimers and trimers, polyesterification operation and refining. Distillation purification operation, etc.

Active Publication Date: 2013-12-04
SHAOXING MINSHENG PHARMA
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  • Summary
  • Abstract
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  • Claims
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Problems solved by technology

The method patented by US20060287543 is: add calcium hydroxide to 5% to 10% liquid methionine aqueous solution, decolorize and filter, add acetone to crystallize, filter and dry to obtain the product, or adjust the liquid methionine aqueous solution to pH with sodium hydroxide aqueous solution The value is about 9, decolorization and purification, adding calcium chloride alcohol solution and then concentrating to obtain calcium salt. Compared with other rough processes, the product purity of this patent is relatively high. However, because only activated carbon decolorization is used for purification, raw materials are not considered The presence of a large number of dimers and trimers (the polymer does not react with calcium hydroxide), so the content of the product is also greatly affected, and its method is also used as a feed additive
In order to avoid the interference of the polymer, the patent CN101348451 esterifies the liquid methionine and then rectifies and purifies the esterified product to obtain a high-purity esterified product, and then forms a salt with calcium hydroxide in a solvent to obtain the product. This method solves the problem of polymer in liquid methionine. The interference of racemic hydroxymethionine calcium that meets the pharmaceutical standard can be prepared, but due to the extra step of esterification operation and rectification purification operation, the steps and difficulty of the operation are increased
And also in order to avoid the influence of the polymer, CN102079719 reacts liquid methionine with ammonia water to generate ammonium salt, then dehydrates to form amide, extracts, concentrates, crystallizes and purifies to obtain high-content amide, and amide is hydrolyzed into 2-hydroxyl-4-methylsulfide by alkali Butyrate, then react with calcium chloride to generate the crude product of racemic hydroxymethionine calcium, and obtain the finished product after refining. This method can also obtain pharmaceutical standard racemic hydroxymethionine calcium, but it also increases the steps of reaction and operation

Method used

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  • Novel method for preparing medicinal despun hydroxyl methionine calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 70kg of liquid methionine, 210kg of pure water, and 2.45kg of sulfuric acid to the reactor in sequence, and heat up to reflux (98-105°C) for 10.0 hours. Cool down to room temperature, add calcium hydroxide to pH 2.5~3.5, add 300kg tetrahydrofuran dropwise at 10~20°C, keep warm for 20~30 minutes after the dropwise addition, press filter, add 120kg pure water to the filtrate, and concentrate the reaction solution under reduced pressure to 350kg (for standby), cool down to below 43°C, weigh, add pure water until the total reaction liquid weighs 420kg. Raise the temperature to 60°C, add calcium hydroxide in batches until the pH is 4.5-5.5, add 1.0 kg of activated carbon, decolorize at 70-80°C for 20-30 minutes, and press filter. The tetrahydrofuran-water mixture obtained by concentration under reduced pressure was slowly added dropwise at 60-64°C. After dripping, the temperature was naturally cooled to room temperature, and the crystal was incubated for 2 hours, and ce...

Embodiment 2

[0029]Add 70kg of liquid methionine, 210kg of pure water, and 3.15kg of sulfuric acid to the reactor in sequence, and heat up to reflux (98-105°C) for 7.0 hours. Cool down to room temperature, add calcium hydroxide to pH 2.5-3.5, add 300kg methanol dropwise at 10-20°C, keep warm for 20-30 minutes after the dropwise addition, press filter, add 120kg pure water to the filtrate, and concentrate the reaction solution under reduced pressure to 320kg (for standby), cool down to below 43°C, weigh, add pure water until the total reaction liquid weighs 480kg. Raise the temperature to 60°C, add calcium hydroxide in batches until the pH is 4.5-5.5, add 1.0 kg of activated carbon, decolorize at 70-80°C for 20-30 minutes, and press filter. The methanol-water mixed solution obtained by concentrating under reduced pressure was slowly added dropwise at 60-64°C. After dripping, the temperature was naturally cooled to room temperature, and the crystal was incubated for 2 hours, and centrifuged...

Embodiment 3

[0032] The difference between this example and Example 2 is that 350kg of acetone is used instead of methanol as the solvent to obtain 68.0kg of refined product, with a loss on drying of 28.0%, a content of 99.5% (area normalization method), and a total yield of 70.6%.

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Abstract

The invention discloses a novel method for preparing medicinal despun hydroxyl methionine calcium. Pure water and acid are added to feed grade liquid methionine to carry out warming and backflow, after cooling, calcium hydroxide is added to the mixture to regulate the pH value, an organic solvent is added to the mixture, a small amount of solid impurities are filtered, vacuum concentration is carried out after adding pure water into the filter liquor, purified water is added, calcium hydroxide is added to the mixture to regulate the pH value after warming, the organic solvent is added to the mixture dropwise after activated carbon decoloration, cooling and centrifugation are carried out after dropwise adding is completed, crude products of the despun hydroxyl methionine calcium are obtained, and the crude products of the despun hydroxyl methionine calcium are refined in a mixed solvent of pure water and the organic solvent to obtain the refined products of the despun hydroxyl methionine calcium. According to the technology, raw materials are easy to obtain, the technology is simple, used solvents can be recycled to use, the content and purity of obtained products are quite high, the crystalline form is quite good, stirring of high rotating speed is not needed, materials are easy to separate and dry, the phenomena of caking and hardening in material drying will not be generated, course products in a mother solution can also be recycled, and the novel method for preparing the medicinal despun hydroxyl methionine calcium is suitable for industrial mass production.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a chemical synthesis method of racemic hydroxymethionine calcium. Background technique [0002] Racemic hydroxymethionine calcium is one of the main components of compound α-keto acid tablets (Kaitong). α-ketoacids and their derivatives have shown increasingly broad application prospects in food, daily chemicals and medicine. In food applications, it can be used as a component of sports nutrition drinks; in functional skin care cosmetics, it can play a very good role in moisturizing, anti-wrinkle, anti-shrinkage, anti-aging and anti-allergy. In medical applications, compound α-ketoacid tablets can treat damage caused by chronic renal insufficiency, and can be used as a specific drug for treating uremia. For patients with renal failure, taking compound α-ketoacid tablets, combined with a low-protein diet, can reduce hyperfiltration of glomeruli and protect nephrons. For p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/58C07C319/20C07C319/28
Inventor 邢亚军傅小明黄希
Owner SHAOXING MINSHENG PHARMA
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