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Method for continuously preparing N-ethyloxyl oxalyl alanine ethyl ester

A technology of ethyl ethoxy oxalyl alanine and diethyl oxalate is applied in the field of continuous preparation of vitamin B6 intermediate - N-ethoxy oxalyl alanine ethyl ester, and can solve the problem of mild reaction conditions , the lack of high yield, etc.

Active Publication Date: 2015-06-24
DAFENG HEGNO PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In summary, this area still lacks a kind of high yield, mild reaction conditions, the preparation method of N-ethoxy oxalylalanine ethyl ester suitable for industrialized production

Method used

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preparation example Construction

[0064] The preparation method of N-ethoxy oxalylalanine ethyl ester

[0065] A kind of method for preparing N-ethoxy oxalylalanine ethyl ester of the present invention is characterized in that, comprises the steps:

[0066] (1) providing a reaction feed liquid, containing alanine, oxalic acid, ethanol and diethyl oxalate in the described reaction feed liquid;

[0067] (2) adding the reaction feed liquid as a reaction system into the reaction device, and reacting in the presence of a water-carrying agent, so that the product water-carrying agent forms a water-water-carrying agent dispersion system; wherein, the water-carrying agent is ethanol;

[0068] (3) steaming out the water-water-carrying agent dispersion system, and removing excess diethyl oxalate to obtain the product N-ethoxy ethyl oxalylalanine.

[0069] The reaction feed solution can be obtained by any conventional method in the art, such as prepared by the following method: mixing alanine, oxalic acid, ethanol and ...

Embodiment approach 1

[0087] Embodiment 1: (3 kettles connected in series, residence time 20h)

[0088] In a 5L reaction flask equipped with mechanical stirring and a thermometer, add 600g of alanine, 933g of oxalic acid, 1551g of absolute ethanol, and 1181g of diethyl oxalate in sequence. To the first bottle in the overflow bottle of three 500ml in series, dissolve and clear the material, the total residence time is 20h, and use another metering pump to beat ethanol in the first overflow bottle with a speed of 2.89g / min simultaneously, The evaporation rate of the first bottle is 2.05g / min, the water content is about 9.5%, and the internal temperature is 90°C. After the bottle is full, it enters the next reaction bottle through overflow, and the evaporation rate of the second bottle is 1.03g / min. min, moisture 6%, internal temperature 94°C, the steaming rate of the third bottle is 0.34g / min, moisture 2%, internal temperature 98°C. And continuously receive the reacted reaction solution from the thi...

Embodiment approach 2

[0089] Embodiment 2 (3 kettles connected in series, residence time 25h)

[0090] In a 5L reaction flask equipped with mechanical stirring and a thermometer, add 600g of alanine, 933g of oxalic acid, 1551g of ethanol, and 1181g of diethyl oxalate in sequence. The first bottle in a 500ml series overflow bottle is used to dissolve and clear the material, and the total residence time is 25h. At the same time, another metering pump is used to beat ethanol in the first overflow bottle at a speed of 2.31g / min. The evaporation rate of the first bottle is 1.64g / min, the water content is about 10%, and the inner temperature is 90°C. After the bottle is full, it enters the next reaction bottle through overflow, and the evaporation rate of the second bottle is 0.82g / min. The water content is 6%, the inner temperature is 94°C, the steaming rate of the third bottle is 0.27g / min, the water content is 2%, and the inner temperature is about 98°C. And continuously receive the reacted reaction ...

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Abstract

The invention discloses a method for continuously preparing N-ethyloxyl oxalyl alanine ethyl ester. The method for continuously preparing the N-ethyloxyl oxalyl alanine ethyl ester concretely comprises the following steps: (1) providing reaction feed liquid, wherein the reaction feed liquid contains alanine, oxalate, ethanol and diethyl oxalate; (2) adding the reaction feed liquid into a reaction device as a reaction system, and carrying out reaction in the presence of a water carrying agent, so that product water and the water carrying agent form a water-water carrying agent dispersion system, wherein the water carrying agent is ethanol; and (3) distilling off the water-water carrying agent dispersion system and removing excessive diethyl oxalate, thus obtaining the N-ethyloxyl oxalyl alanine ethyl ester product. The method for continuously preparing the N-ethyloxyl oxalyl alanine ethyl ester has the advantages that continuous and automatic production can be realized, and hypertoxic benzene is not used, so that the method for continuously preparing the N-ethyloxyl oxalyl alanine ethyl ester is more environmental-friendly; meanwhile, reaction time is short and energy consumption is low.

Description

technical field [0001] The invention relates to the technical field of vitamin production, in particular to a continuous preparation method of vitamin B6 intermediate-N-ethoxy ethyl oxalylalanine. Background technique [0002] Vitamin B6 is one of the essential vitamins for the human body, which plays a vital role in the regulation of various physiological functions of the human body and growth and development. Vitamin B6 can maintain the balance of sodium and potassium in body fluids, regulate body fluids, and participate in the production of red blood cells. Therefore, it is often used in the treatment of vitamin B6 deficiency in the human body and adjuvant treatment of other diseases, and can also be used as food additives. [0003] Ethyl N-ethoxy oxalylalanine is an important intermediate for the preparation of vitamin B6. At present, the disclosed methods for preparing this intermediate mainly include: [0004] The method disclosed in US3646061 is to react alanine, oxa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/56C07C231/02B01J19/00
Inventor 刘德铭鲁向阳陈常见徐光明
Owner DAFENG HEGNO PHARMA
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