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Method for preparing pyruvate ester

A technology of pyruvate and lactate, which is applied in the field of solid-liquid phase reaction system to prepare pyruvate, can solve the problems of environmental pollution, difficult product purification, and many reaction by-products, and achieves simple and easy-to-operate, high-efficiency Effect of pyruvate selectivity and high lactate conversion

Inactive Publication Date: 2014-02-12
CHINA PETROCHEM DEVMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature Beilsteins Handbuch der Organischer Chemie, vol. III, 4 th Supplement, p.1513 mentions that potassium permanganate or potassium permanganate plus copper sulfate can be used to catalyze the oxidation of lactate to prepare pyruvate, but potassium permanganate has strong oxidative properties and many reaction by-products, which lead to The product is not easy to purify, the yield is poor, and potassium permanganate will cause serious environmental pollution
There is incomplete oxidation of lactic acid ester in the above-mentioned method, the shortcoming that productive rate is low
[0005] In addition, the problem of preparing pyruvate by direct oxidation of lactate is that the carbon-carbon single bond of lactate is easily broken to generate aldehyde and carbon dioxide, which in turn affects the yield of pyruvate and subsequent purification and separation.

Method used

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  • Method for preparing pyruvate ester
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  • Method for preparing pyruvate ester

Examples

Experimental program
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Effect test

preparation example 1

[0020] Preparation Example 1 The preparation of titanium-silicon molecular sieve

[0021] The titanium-silicon molecular sieves used in the following reactions are all prepared in this way.

[0022] First, 1.98 g of tetra-n-butyl titanate was added to a 500 ml round bottom flask equipped with a vacuum system and an isobaric feeding system, and nitrogen blanketing was carried out. The nitrogen-covered round-bottom flask was cooled to 5° C., and after the temperature was balanced, 30 g of tetraethylsilicate was added dropwise into the nitrogen-covered round-bottom flask using the isobaric feeding system. After the dropwise addition was complete, stir at 5° C. for 1 hour. Afterwards, get the isopropanol solution (20% by weight) of the tetra-n-propylammonium hydroxide of 56 grams, use this isobaric feeding system to add dropwise in this nitrogen-covered round-bottomed flask equally, treat to drop after finishing and finish in 5 Stir for 1 hour at °C. Next, 44.8 g of water was a...

Embodiment 1 to 2

[0024] The purpose of Examples 1 to 2 is to screen the reaction solvent. Add 1 gram of the titanium-silicon molecular sieve of Preparation Example 1 in a 250 milliliter three-necked round-bottomed flask equipped with a condenser tube and a stirring system according to the contents recorded in Table 1, and 20 grams of the titanium-silicon molecular sieve as listed in Table 1. 2 solvent, and 5 g of ethyl lactate as a reactant. After the reaction temperature was raised to 70° C., 4.11 grams of hydrogen peroxide aqueous solution (35% by weight) was gradually added over the reaction time to carry out the preparation reaction of ethyl pyruvate. After completing the hydrogen peroxide feed for 1 hour, continue to react at this temperature for 5 hours. After the reaction is terminated, the titanium-silicon molecular sieve catalyst is separated from the reaction solution by filtration, and each reaction solution after the separation is separated by gas chromatography. (Varian CP-3800, ...

Embodiment 3 to 7

[0039] The purpose of Examples 3 to 7 is to adjust the reaction temperature. Add 1 gram of the titanium-silicon molecular sieve of Preparation Example 1, 20 grams of tert-butanol as a solvent, and 5 grams of lactic acid in a 250 milliliter three-necked round-bottomed flask equipped with a condenser tube and a stirring system according to the contents shown in Table 3 respectively. Ethyl esters were used as reactants. After raising the reaction temperature to the temperature shown in Table 3, 4.11 g of hydrogen peroxide aqueous solution (35% by weight) was gradually added over the reaction time to carry out the preparation reaction of ethyl pyruvate. After completing the hydrogen peroxide feed for 1 hour, continue to react at this temperature for 5 hours. After the reaction is terminated, the titanium-silicon molecular sieve catalyst is separated from the reaction solution by filtration, and the separated reaction solutions are subjected to gas chromatography. and titrator ana...

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Abstract

A method for preparing a pyruvate ester is disclosed. In the method of the present invention, a lactate ester is oxidized by hydrogen peroxide in the presence of a Ti-Si molecular sieve catalyst. In the present invention, the Ti-Si molecular sieve catalyst is easily filtered and recycled, the reaction conditions are mild due to the usage of hydrogen peroxide, the process is simple and easily performed, the conversion rate of the lactate ester is high, and the selectivity of the pyruvate ester is high.

Description

technical field [0001] The invention relates to a method for preparing pyruvate, in particular to a method for preparing pyruvate in a solid-liquid phase reaction system using titanium-silicon molecular sieves and an oxidizing agent. Background technique [0002] Pyruvate is an important intermediate in organic synthesis and is widely used in industries such as medicine, pesticide, fragrance, cosmetics and laser raw materials. At present, there are two main methods for producing pyruvate in industry. One is to esterify tartaric acid after dehydration. Under easy hydrolysis, the reaction yield is low. Therefore, in the development of pyruvate preparation methods, the preparation of high-purity products and mild reaction conditions are necessary. [0003] There are many methods and raw materials for synthesizing pyruvate, among which the synthesis method using lactic acid ester as raw material is the simplest and most effective reaction route, which is mainly divided into ga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/313
CPCC07C67/313C07C69/716
Inventor 施建全谢正发方顺一
Owner CHINA PETROCHEM DEVMENT
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