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Method for preparing N-ethoxy oxalyl-alanine ethyl ester

A technology of ethyl alanine and oxalyl alanine, which is applied in the field of preparation of vitamin B6 intermediate——N-oxalyl ethoxy-ethyl alanine, which can solve the problems of cumbersome process steps, equipment corrosion, N-ethoxyoxalyl-alanine ethyl ester cannot be applied, etc., to achieve the effect of simple process and material saving

Inactive Publication Date: 2004-01-28
CHANGSHU CHEM JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, the process steps are more cumbersome
Therefore transplant to prepare N-ethoxy oxalyl-alanine ethyl ester with this method and can't be applicable
[0006] CN86101512 relates to a vitamin B e The synthesis process of the intermediate 4-methyl-5-alkoxy oxazole, in which hydrochloric acid is used as a catalyst, not only causes corrosion to equipment, but also brings environmental problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 2000ml three-neck flask, add 356 grams of α-alanine, 1080 grams of oxalic acid, 1070 grams of 95% ethanol, and 800 grams of benzene, install a stirring and distillation water separation device, then heat to dissolve, and heat to 75 ° C under stirring ~80°C. After the water in the distillate was separated, the benzene layer was returned to the reaction flask. When the reaction time reaches 60 hours, extract the reaction feed liquid to measure the moisture content, and when the feed liquid contains less than 0.5%, it is the end of the reaction. Then heating and steaming out the benzene that can be used again, the ethanol and the diethyl oxalate generated to obtain N-ethoxyoxalyl-alanine ethyl ester. The equation for the above reaction is as follows: α-Alanine Oxalic acid Ethanol N-ethoxyoxalyl-alanine ethyl ester

[0019] Among them, α-alanine can be L-type, or D, L-type, it can be used first to form alanine oxalate with oxalic acid; diethyl oxalate can be ...

Embodiment 2

[0021] In a 2000ml three-neck flask, add 356 grams of α-alanine, 650 grams of oxalic acid, 900 grams of 95% ethanol, 800 grams of benzene, and 500 grams of diethyl oxalate, install a stirring and distillation water separator, then heat to dissolve, Heat to 75°C to 80°C while stirring. After the water in the distillate was separated, the benzene layer was returned to the reaction flask. When the reaction time reaches 60 hours, extract the reaction feed liquid to measure the moisture content, and when the feed liquid contains less than 0.5%, it is the end of the reaction. Then heating and distilling out the reusable benzene and unreacted ethanol and the generated diethyl oxalate to obtain N-ethoxyoxalyl-alanine ethyl ester. The remaining descriptions in this embodiment are the same as those in Embodiment 1.

Embodiment 8

[0023] In a 2000ml three-neck flask, add 356 grams of α-alanine, 650 grams of oxalic acid, 855 grams of absolute ethanol, 700 grams of benzene, and 500 grams of diethyl oxalate, install a stirring and distillation water separator, and then heat until dissolved. Heat to 75°C to 80°C while stirring. After the water in the distillate was separated, the benzene layer was returned to the reaction flask. When the reaction time reaches 60 hours, extract the reaction feed liquid to measure the moisture content, and when the feed liquid contains less than 0.5%, it is the end of the reaction. Then heating and steaming out the benzene that can be used again, the ethanol and the diethyl oxalate generated to obtain N-ethoxyoxalyl-alanine ethyl ester. The remaining descriptions in this embodiment are the same as those in Embodiment 1.

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Abstract

The preparation method of N-ethoxyoxalyl-alanine ethyl ester which is intermediate body for producing vitamin B6 is characterized by that it uses benzene as dewatering agent, and in the system of alpha-alanine, oxalic acid, ethyl alcohol, diethyl oxalate and benzene and under the condition of heating reaction it can continuously remove water content from said system, and can adopt one-step process to implement esterification and acylation of alpha-alanine to obtain the invented N-ethoxyoxalyl-alanine ethyl ester.

Description

technical field [0001] The present invention relates to a method for producing vitamin B 6 Intermediate - the preparation method of N-ethoxyoxalyl-alanine ethyl ester. Background technique [0002] Vitamin B 6 It is a necessary substance for the human body and animals to maintain normal physiological functions. It participates in the metabolism of amino acids and proteins in the body. Therefore, it is used as vitamin B in humans and animals 6 Auxiliary therapeutic drugs and food and feed additives for deficiency or other diseases. [0003] Currently, vitamin B 6 The preparation method widely adopts the oxazole process, in the oxazole process, the intermediate N-ethoxyoxalyl-alanine ethyl ester is synthesized from the starting material α-alanine, generally under the catalysis of hydrochloric acid or hydrochloric acid-phosphoric acid Realize the esterification of alanine, then realize the oxalylation of amino group in the presence of acid-removing agent, its main reaction...

Claims

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Application Information

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IPC IPC(8): C07C231/10C07C235/80
Inventor 王祥忠
Owner CHANGSHU CHEM JIANGSU
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