Process method for preparing sodium 2-ketobutyrate

A process method and technology of sodium butanone, applied in the field of preparing 2-butanone sodium salt, can solve the problems of difficulty in scaling up to kilograms and ten kilograms, expensive Grignard reagents, harsh reaction conditions, etc., and avoid dangerous and expensive Reagents, to meet large-scale industrial production, the effect of mild reaction conditions

Active Publication Date: 2020-05-12
SUZHOU BAILINGWEI HYPERFINE MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, this method also has two serious problems. The first is that the reaction conditions are very harsh and must be minus 78 degrees. The second is that the Grignard reagent is relatively expensive, and the reactivity is very high, which is relatively dangerous.
These two problems also make it more difficult for this product to be further scaled up in kilograms and ten kilograms
[0007] In order to solve the problems of harsh reaction conditions, high synthesis cost and high risk of reaction in the existing process route of 2-butanuonic acid sodium salt, a safe and reliable 2-butanuonic acid sodium salt with reasonable route design and controllable cost was sought Synthetic methods are of great importance

Method used

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  • Process method for preparing sodium 2-ketobutyrate
  • Process method for preparing sodium 2-ketobutyrate
  • Process method for preparing sodium 2-ketobutyrate

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Embodiment 1

[0044]

[0045] S1: Preparation of 1-carbonylpropane-1,2,2-tricarboxylic acid triethyl ester intermediate

[0046]

[0047] Under stirring at room temperature, 25 L of tert-butyl methyl ether, 8.7 Kg of diethyl methylmalonate and 7.5 Kg of diethyl oxalate were successively added into a 50 L glass reactor, and stirred evenly.

[0048]Further, 0.4Kg of sodium ethoxide was added in batches, and after the addition, the reaction solution was stirred at room temperature for 6 hours, and GC (gas chromatography) confirmed that the reaction was complete.

[0049] Further, hydrogen chloride ethanol solution was added dropwise to the reaction solution to adjust the pH of the reaction solution to 7.

[0050] Further, the reaction solution was first distilled under normal pressure to recover the solvent, and then distilled under reduced pressure to collect 11.8 Kg of 1-carbonylpropane-1,2,2-tricarboxylate triethyl intermediate in the form of yellow liquid, with a yield of 86%.

[00...

Embodiment 2

[0068]

[0069] S1: Preparation of 1-carbonylpropane-1,2,2-tricarboxylic acid trimethyl ester intermediate

[0070]

[0071] Under stirring at room temperature, 25L of tetrahydrofuran, 4.4Kg of dimethyl methylmalonate and 7.1Kg of dimethyl oxalate were successively added into a 50L glass reactor, and stirred evenly.

[0072] Further, 0.3Kg of sodium methoxide was added in batches. After the addition, the reaction solution was heated to 50° C., kept stirring for 5 hours, and GC (gas chromatography) confirmed that the reaction was complete.

[0073] Further, methanolic hydrogen chloride solution was added dropwise to the reaction solution to adjust the pH of the reaction solution to 7.

[0074] Further, the reaction liquid is firstly recovered by normal pressure distillation to recover the solvent, then the excess dimethyl oxalate is recovered by vacuum distillation, and then 6.4Kg of yellow liquid 1-carbonylpropane-1,2,2-tricarboxylic acid tricarboxylate is collected by v...

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Abstract

The invention discloses a process method for preparing sodium 2-ketobutyrate. The method comprises the following steps: S1, reacting diethyl methylmalonate or dimethyl methylmalonate used as a raw material with diethyl oxalate or dimethyl oxalate under the catalysis of a proper amount of an alkaline compound to obtain a 1-carbonyl propane-1,2,2-tricarboxylate intermediate; S2, reacting the 1-carbonyl propane-1,2,2-tricarboxylate intermediate obtained in step S1 with water under the catalysis of a proper amount of an acidic compound to obtain 2-ketobutyric acid; and S3, reacting the 2-ketobutyric acid obtained in step S2 with the alkaline compound to obtain the sodium 2-ketobutyrate. The method is reasonable in route design, safe, reliable, low in cost and capable of achieving quantitativeproduction.

Description

technical field [0001] The invention relates to the field of preparation of diagnostic reagent-2-butanuate sodium salt, in particular to a process for preparing 2-butanuate sodium salt. Background technique [0002] The sodium salt of 2-butanuate is an important diagnostic reagent and a substrate for the detection of α-hydroxybutyrate dehydrogenase, and it can also be used in the synthesis of antiviral agent 6-azapyrimidine-2′-deoxy-4 '-thionucleosides. The detection results of α-hydroxybutyrate dehydrogenase by the kit configured with 2-butyruvate sodium salt are clinically used as the basis for the diagnosis of various diseases such as liver cirrhosis and leukemia. [0003] There are many synthetic routes reported for 2-butanuonic acid sodium salt, but there is only one that can be scaled up to ten grams, which is the following synthetic route reported in patent CN103073411A: [0004] [0005] This route uses dimethyl oxalate as the starting material, reacts with ethy...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C59/185
CPCC07C51/412C07C67/343C07C51/09C07C59/185C07C69/716
Inventor 陈丕证龙韬顾扬邹增龙
Owner SUZHOU BAILINGWEI HYPERFINE MATERIAL
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