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Novel method for synthesizing ethyl pyruvate

A technology of ethyl pyruvate and synthesis method, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of incomplete oxidation of ethyl lactate, difficulty of ethyl pyruvate, low product purity, etc. The problem is to achieve the effect of reasonable ratio of reaction raw materials, simple and easy operation, and high purity.

Inactive Publication Date: 2010-06-16
大连凯飞精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Taking ethyl lactate as raw material synthesis method at present, mainly adopts NO Oxidation method, potassium permanganate oxidation method, sodium hypochlorite oxidation method, ferrous sulfate hydrogen peroxide oxidation method etc., the feature is convenient and fast, but these oxidation methods ethyl lactate oxidation are not Thoroughly, the yield is low, because the boiling point difference of raw material ethyl lactate and ethyl pyruvate is not big, it is difficult to obtain high-purity ethyl pyruvate, and the product purity is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The synthesis method of ethyl pyruvate, the specific process is: in a 500ml four-necked bottle, add 50g ethyl lactate, 37.5g sodium bicarbonate, 0.75g catalyst 2,2,6,6-tetramethylpiperidine nitrogen oxide, 250 g of dichloromethane. Stir mechanically and cool down in an ice-water bath. Add 37.5g oxidant trichloroisocyanuric acid (TCCA) in batches, keep the temperature in the reactor at 14-15°C, after adding TCCA, keep the temperature in the reactor at 13-15°C, and take samples for analysis (GC) after 2 hours of reaction, lactic acid Ethyl ester content < 0.5%, stop stirring. Filter the reaction liquid, wash the filter cake with dichloromethane, combine the filtrates, distill the dichloromethane from the filtrate under atmospheric pressure, and then collect fractions by distillation under reduced pressure to obtain ethyl pyruvate with a content of more than 99%.

Embodiment 2

[0017] The synthesis method of ethyl pyruvate, the specific process is: in a 500ml four-neck bottle, add 50g of ethyl lactate, 40g of sodium bicarbonate, 0.5g of catalyst methylmorpholine nitrogen oxide, and 250g of dichloroethane. Stir mechanically and cool down in an ice-water bath. Add 40g of oxidizing agent TCCA in batches, keep the temperature in the reactor at 14-15°C, after adding TCCA, keep the temperature in the reactor at 13-15°C, take samples for analysis (GC) after 2 hours of reaction, if the content of ethyl lactate is less than 0.5%, stop Stir. Filter the reaction liquid, wash the filter cake with dichloromethane, combine the filtrates, distill the dichloromethane from the filtrate under atmospheric pressure, and then collect fractions by distillation under reduced pressure to obtain ethyl pyruvate with a content of more than 99%.

Embodiment 3

[0019] The synthesis method of ethyl pyruvate, the specific process is: in a 500ml four-necked bottle, add 50g of ethyl lactate, 40g of sodium bicarbonate, 1.0g of catalyst pyridine nitrogen oxide, and 250g of dichloroethane. Stir mechanically and cool down in an ice-water bath. Add 50g of oxidizing agent TCCA in batches, keep the temperature in the reactor at 14-15°C, after adding TCCA, keep the temperature in the reactor at 13-15°C, take samples for analysis (GC) after 2 hours of reaction, if the content of ethyl lactate is less than 0.5%, stop Stir. The reaction liquid was filtered, the filter cake was washed with dichloromethane, the filtrates were combined, the dichloromethane was distilled off from the filtrate by normal pressure distillation, and then the fractions were collected by vacuum distillation to obtain ethyl pyruvate with a content of more than 99%.

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Abstract

The invention relates to a method for synthesizing an organic compound. The method for synthesizing ethyl pyruvate adopts ethyl lactate and sodium hydroxide bicarbonate as raw materials, and the raw materials of ethyl lactate and sodium bicarbonate are prepared according to certain mole ratios and are processed by synthetic reaction in an organic solvent under the existence of an oxynitride catalyst and oxidizer trichloroisocyanuric acid; and after reaction, reaction liquid is processed by filtration, solvent removal, pressure reduction and distillation and then is collected to obtain the ethyl pyruvate product. Compared with the traditional method, the method for synthesizing the ethyl pyruvate is outstandingly characterized by reasonable proportion of reaction raw materials, simple and easily operated process, nearly 100 percent of percent conversion of the raw materials by particularly adopting the novel catalyst oxynitride and the oxidizer trichloroisocyanuric acid (TCCA), capability of quantitative reaction and high purity and yield of products obtained by reaction, thereby meeting the requirement of each industry on application.

Description

1. Technical field: [0001] The present invention relates to a method for synthesizing organic compounds. 2. Background technology: [0002] Ethyl pyruvate, also known as Ethyl 2-oxopropionate, Brenztraubensaeure-ethylester, has a molecular formula of C5H8O3. [0003] Ethyl pyruvate is an important intermediate in organic synthesis and is widely used in industries such as medicine, cosmetics, pesticides, spices and laser materials. As a pharmaceutical intermediate, it can be used to synthesize drugs such as cardiovascular dilators; it can be used in cosmetics for whitening and nourishing skin, it can promote skin wound healing, prevent and treat skin diseases characterized by cracking, peeling and scaling; it can be used as air The high-efficiency active ingredient in the freshener can effectively remove ammonia and methyl mercaptan in the air; ethyl pyruvate itself has a special fragrance, so it can be used in flavors and fragrances; at the same time, ethyl pyruvate is also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/738C07C67/313B01J31/02
Inventor 秦学孔高崇王延波冯承刚
Owner 大连凯飞精细化工有限公司
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