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Method for synthesizing high-purity 2-ketonate

A keto acid salt, high-purity technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, fermentation and other directions, can solve the problems of cumbersome chemical treatment steps, large amount of organic solvent, unfavorable industrial production, etc. The effect of mild conditions, lower production costs, and environmental protection in the production process

Active Publication Date: 2015-02-25
HUNAN BAOLISHI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The method for synthesizing keto acid salts by existing chemical methods has low yield, difficult purification, large amount of organic solvent used, difficult recovery, resulting in high cost, environmental pollution, and cumbersome chemical treatment steps, which are not conducive to industrial production, etc. The defect of; the purpose of the present invention is to provide a kind of simple operation, mild reaction conditions, low cost, high yield to prepare the method for high-purity 2-keto acid salt

Method used

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  • Method for synthesizing high-purity 2-ketonate
  • Method for synthesizing high-purity 2-ketonate
  • Method for synthesizing high-purity 2-ketonate

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Take 35.7 grams of glycine (anhydrous) and add an appropriate amount of deionized water to dissolve it, add 40% 45.74mL of acetaldehyde solution, dissolve it with 3.0mol / L sodium hydroxide solution and control the pH at about 7.50, and vacuum filter to remove the insoluble and dilute to 600mL. Input L-threonine aldolase by 30000U / L (wherein U is the total enzyme activity of enzyme input, L is the reaction volume) ratio and by 20000U / L (wherein U is the total enzyme activity of enzyme input, L is Reaction volume) ratio into L-threonine deaminase, control reaction temperature 30 ℃, keep pH at 7.50 with 3.0mol / L sodium hydroxide solution in the reaction process, stop reaction when liquid phase glycine remains below 0.2%, The transformation stop solution was filtered off. 624 mL of a solution containing 45.80 g of 2-butanuonic acid was obtained, and the yield was 98.0%. Put the conversion termination liquid directly on the 200mL ion exchange chromatography column regenera...

Embodiment 2

[0048] Take 37.8 grams (anhydrous) glycine and add appropriate amount of deionized water to dissolve it, then add 97% 35.6mL propionaldehyde solution, dissolve it with 3.0mol / L sodium hydroxide solution and control the pH at about 7.50, vacuum filter to remove insoluble matter , and set the volume to 600mL. Add 30000U / L of L-threonine aldolase and 20000U / L of L-threonine deaminase, control the reaction temperature at 30°C, and keep the pH at 7.50±0.05 with 3.0mol / L sodium hydroxide. When the conversion rate was greater than or equal to 99%, the conversion-terminated solution was filtered out to obtain 626 mL of a solution containing 54.73 g of 2-pentanuonic acid, with a yield of 98.3%. Put the conversion termination liquid directly on the 200mL ion exchange chromatography column regenerated by hydrochloric acid, the flow rate is: 6.67mL / min (2.0Bv / h). Directly use deionized water as the eluent to collect 2-pentanuonic acid, the range of collected liquid is 120-815 mL, the vol...

Embodiment 3

[0050] Take 34.0 grams of glycine (anhydrous) and add an appropriate amount of deionized water to dissolve it, then add 40% 52.4 mL of acetaldehyde solution, dissolve it with 3.0 mol / L sodium hydroxide solution and control the pH at about 7.50, and vacuum filter to remove the insoluble and dilute to 600mL. Add L-threonine aldolase at a ratio of 40000U / L and L-threonine deaminase at a ratio of 20000U / L, control the reaction temperature at 30°C, and use 3.0mol / l sodium hydroxide solution during the reaction Keep the pH at 7.50, terminate the reaction when the glycine in the liquid phase remains below 0.2%, and filter out the conversion termination solution. 644 mL of a solution containing 44.08 g of 2-butanuonic acid was obtained, and the yield was 94.3%. Put the conversion termination liquid directly on the 200mL ion exchange chromatography column regenerated by hydrochloric acid, the flow rate is: 6.67mL / min (2.0Bv / h). Directly use deionized water as the eluent to collect 2-...

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Abstract

The invention discloses a method for synthesizing high-purity 2-ketonate. The method comprises the following steps: carrying out an enzyme catalysis reaction on an aldehyde compound and a glycine raw material in the catalysis of L-threonine aldolase and L-threonine deaminase compound enzyme to generate a 2-ketonic acid product; carrying out separation purification on the 2-ketonic acid product by chromatography, adjusting the pH to a proper value by adopting alkali carbonate or alkali hydrocarbonate, and sequentially carrying out actived carbon decoloration, concentration crystallization and vacuum drying to obtain 2-ketonate. The preparation method has the advantages of simplicity in operation and mild reaction condition, does not cause pollution by adopting an aqueous phase system, and has low production cost; prepared 2-ketonate has high yield and high purity.

Description

technical field [0001] The invention relates to a method for synthesizing 2-keto acid by a novel biological method and separating and purifying it to obtain a pharmaceutical grade keto acid salt, which belongs to the field of biosynthesis. Background technique [0002] 2-keto acid salts are mainly used in biochemical reagents, in vitro diagnostics, and cosmetic additives. In addition, they are also important pharmaceutical intermediates, mainly used in dietary supplements for fitness and weight loss. Kits configured with 2-butyruvate are widely used in the detection of α-hydroxybutyrate dehydrogenase, and are used as diagnostic basis for myocardial infarction, anemia, leukemia, liver cirrhosis and other diseases. Sodium pyruvate is the substrate for the determination of lactate dehydrogenase, and it is mainly used for the determination of glutamate-alanine aminotransferase activity in liver function tests. Sodium 2-pentanoate is mainly used for hypocalcemia, urticaria, angi...

Claims

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Application Information

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IPC IPC(8): C12P7/40
CPCC07C51/42C12P7/40C07C59/185
Inventor 许岗曾红宇王胜锋帅得利
Owner HUNAN BAOLISHI BIOTECH
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