Synthesis preparation method of pyruvate

A technology of pyruvate and lactate, applied in the field of pyruvate synthesis and preparation, can solve the problems of low yield, unfriendly environment, complicated post-processing and the like, and achieves the effects of mild reaction temperature, small safety risk and environmental friendliness

Inactive Publication Date: 2019-08-06
HUBEI LANSUN BIOCHEM PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional synthesis process is to synthesize ethyl pyruvate by dehydration and decarboxylation of tartrate diester, but this method has the characteristics of low yield, complicated post-treatment, and serious environmental pollution.
With the active development of "Green Chemistry" today, seeking a high-yield, highly operable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0022] Example 1

[0023] In the embodiment of the present invention, ethyl lactate is used as the lactate, dichloromethane is used as the solvent, dichloroisocyanuric acid is used as the oxidant, and sodium bicarbonate is used as the base.

[0024] A synthetic preparation method of pyruvate includes the following steps:

[0025] S10: Dissolve 118g (1.0mol) of ethyl lactate in 590ml of dichloromethane to obtain an ethyl lactate solution;

[0026] S20, add 0.35g 2,2,6,6-tetramethylpiperidine nitrogen oxide and 109.2g (1.3mol) sodium bicarbonate to the lactate solution, mix and stir for 1-3h at 10-20℃ , Get a mixed solution;

[0027] S30: Add 124.8g (0.63mol) of dichloroisocyanuric acid to the mixed solution and mix and stir to react. The temperature is controlled within 18-23°C and the stirring time is 3-5h. After the reaction is over, the temperature is reduced to 10-20°C. Get semi-finished products

[0028] S40, filtering the semi-finished products and collecting the filtrate;

[0029]...

Example Embodiment

[0032] Example 2

[0033] In the embodiment of the present invention, methyl lactate is used as the lactate, 1,2-dichloroethane is used as the solvent, dichloroisocyanuric acid is used as the oxidant, and sodium bicarbonate is used as the base.

[0034] A synthetic preparation method of pyruvate includes the following steps:

[0035] S10: Dissolve 104g (1.0mol) of methyl lactate in 590ml of 1,2-dichloroethane to obtain a methyl lactate solution;

[0036] S20, add 0.45g 2,2,6,6-tetramethylpiperidine nitrogen oxide and 116g (1.5mol) sodium bicarbonate to the lactate solution, mix and stir for 1-3h at 20-30℃, Get a mixed solution;

[0037] S30: Add 99g (0.5mol) of dichloroisocyanuric acid to the mixed solution, mix and stir for reaction, control the temperature within 20-30°C, and stir for 3-5h. After the reaction is over, cool down to 10-20°C to obtain Semi-finished products

[0038] S40, filtering the semi-finished products and collecting the filtrate;

[0039] S50, recover the residual ...

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PUM

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Abstract

The invention discloses a synthesis preparation method of a pyruvate, and belongs to the chemical field. The synthesis preparation method comprises following steps: S10, a lactate s dissolved in a solvent so as to obtain a lactate solution; S20, a catalyst and an alkali are added into the lactate solution so as to obtain a semi-finished product; S40, the semi-finished product is subjected to filtering, and an obtained filtrate is collected; S50, the solvent is recycled, underpressure distillation is carried out, and distillation fractions are collected so as to obtain a finished product. According to the synthesis preparation method, no bromine or dangerous peroxide is adopted, and at the same time, no dangerous illumination operation is needed; reaction temperature is mild; after reaction, only filtering solid liquid separation is needed; no waste liquid is generated; after filtrate solvent recycling, high purify product can be obtained only through distillation; reaction conversion rate is 95% or higher; product GC purity is as high as 98% or higher; product yield is 90% or higher; safety risk is low; the synthesis preparation method is friendly to the environment, and is suitable for industrialized large scale production.

Description

Technical field [0001] The invention relates to the field of chemical engineering, in particular to a synthetic preparation method of pyruvate. Background technique [0002] Ethyl pyruvate is an important organic intermediate. Because of its bifunctional group and more reaction centers, it shows more important and special chemical properties than general compounds. Ethyl pyruvate is widely used in biology, medicine, food, perfume and cosmetics. Because of its active chemical properties, difficult preparation, and extremely wide and important uses, actively exploring new synthetic methods has become a hot spot for many chemists. [0003] The traditional synthesis process uses tartrate diester dehydration and decarboxylation to synthesize ethyl pyruvate, but this method has the characteristics of low yield, complex post-processing, and serious environmental pollution. Today, with the active development of "green chemistry", seeking a synthetic route with high yield, strong operabil...

Claims

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Application Information

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IPC IPC(8): C07C67/313C07C69/716
CPCC07C67/313
Inventor 叶澜杰忠义
Owner HUBEI LANSUN BIOCHEM PHARMA
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