Ketobutyric acid and preparation method for ketobutyric acid salt

Abstract

The invention provides an Alpha-ketobutyric acid preparation method which comprises the following steps: A), taking dimethyl oxalate or diethyl oxalate as raw materials to solve in anhydrous furanidine, cooling, adding ethylmagnesium bromide solution, stirring, removing solvent through distillation under reduced pressure after reaction termination, allowing residual mixture to be subjected to rectification under reduced pressure, and collecting intermediate product 2-oxo methyl butyrate or 2-oxo ethyl butyrate; B), solving the intermediate product in a hydrochloric acid, heating, reflowing, stirring, performing extraction by vinegar naphtha after the completion of the reaction, collecting organic phase, drying, filtering, and removing the solvent through allowing the filtrate to be subjected to distillation under reduced pressure, so as to obtain a coarse product Alpha-ketobutyric acid; and c), allowing the coarse product Alpha-ketobutyric acid to be subjected to rectification under the reduced pressure, and collecting the Alpha-ketobutyric acid. The method provided by the invention has the advantages of inexpensive and easy-to-get raw materials, lower toxicity, simple preparation process, easiness in control, no complex purification process, high product purity, high productivity, and greatly reduced manufacturing cost, and is suitable for large scale industrialized application.

Description

technical field [0001] The invention relates to a preparation method of butyronic acid and its salt. Background technique [0002] 2-butyronic acid (also known as: α-ketobutyric acid) and its sodium salt can be used in biochemical research, diagnostic reagents and other fields, and is the substrate of α-hydroxybutyrate dehydrogenase. Kits prepared from 2-butyronic acid are widely used in the detection of α-hydroxybutyrate dehydrogenase in clinical practice, and are used as the basis for the diagnosis of potential diseases such as myocardial infarction, anemia, leukemia, and liver cirrhosis. The 2-butanuonic acid currently used is all dependent on imports, and the preparation cost is high, resulting in high testing costs for patients. [0003] An existing method for preparing 2-butanone acid is to use 2-butynoic acid as the starting material, mix it with ruthenium trichloride, adjust the pH value, heat to 100°C and stir the reaction, and concentrate to obtain the product aft...

AI Technical Summary

Problems solved by technology

The preparation method lacks sources of starting materials, is volatile, difficult to store, and highly toxic; the reaction conditions are difficult to control, the product is difficult to purify, the yield is low, and the preparation cost is high

[0004]Another 2-butanuonic acid preparation method uses butadiene as a raw material, through catalytic oxidation, there may be a small amount of 2-butanol in its by-products Keto acids and other organic acids, the selectivity of the reaction is not high, the yield is low, and the product purification is difficult

[0005]Therefore, the existing 2-butanuonic acid preparation method has the shortage of raw material sources, difficult product purification, low yield, and high preparation costs, which are unfavorable for large-scale production. Industrial production and wide application

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