Check patentability & draft patents in minutes with Patsnap Eureka AI!

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 alanine-ethyl alanine, can solve equipment corrosion, cumbersome process steps, N - Problems such as the inapplicability of oxalyl-alanine ethyl ester to achieve the effect of saving materials and simple process

Inactive Publication Date: 2005-03-16
CHANGSHU CHEM JIANGSU
View PDF3 Cites 2 Cited by
  • 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
[0007] CN86101512 relates to a vitamin B 6 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing N-ethoxy oxalyl-alanine ethyl ester
  • Method for preparing N-ethoxy oxalyl-alanine ethyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a 2000ml three-necked 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, the reaction feed liquid is extracted to measure the water content. When the feed liquid contains less than 0.5% of water, it is the reaction end point. Then heating and steaming the benzene available for recycling, unreacted ethanol and the generated diethyl oxalate to obtain N-ethoxyoxalyl-alanine ethyl ester. The equation for the above reaction is as follows:

[0018]

[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 generated by oxalic acid and ethanol in the system...

Embodiment 2

[0021] In a 2000ml three-necked flask, add 356 grams of α-alanine, 650 grams of oxalic acid, 900 grams of 95% ethanol, 800 grams of benzene, 500 grams of diethyl oxalate, install a stirring and distilled water separation device, and then heat until dissolved, Heat to 75°C to 80°C with stirring. After the water in the distillate was separated, the benzene layer was returned to the reaction flask. After the reaction times reached 60 hours, the reaction feed liquid was extracted to measure the moisture content, and when the feed liquid contained water (0.5%), it was the reaction end point. Then the benzene and unreacted ethanol and the oxalic acid generated by heating were steamed out for reuse. Diethyl ester, namely N-ethoxyoxalyl-alanine ethyl ester. Remaining description in this embodiment is the same as embodiment 1.

Embodiment 3

[0023] In a 2000ml three-necked flask, add 356 grams of α-alanine, 650 grams of oxalic acid, 855 grams of absolute ethanol, 700 grams of benzene, 500 grams of diethyl oxalate, install a stirring and distilled water separator, and then heat until dissolved, Heat to 75°C to 80°C with 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, the reaction feed liquid is extracted to measure the water content. When the feed liquid contains less than 0.5% of water, it is the reaction end point. Then heating and steaming the benzene available for recycling, unreacted ethanol and the generated diethyl oxalate to obtain N-ethoxyoxalyl-alanine ethyl ester. The rest of the descriptions in this embodiment are the same as those in Embodiment 1.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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 kind of production of vitamin B 6 The preparation method of intermediate - N-ethoxyoxalyl-alanine ethyl ester. Background technique [0002] Vitamin B 6 It is a necessary substance for human and animals to maintain normal physiological functions, and it participates in the metabolism of amino acids and proteins in the body. Therefore, it is used as human and animal vitamin B 6 Drugs for adjuvant therapy and food and feed additives for deficiency or other diseases. [0003] Currently, vitamin B 6 The preparation method of oxazole is widely used. In the oxazole process, the intermediate N-ethoxyoxalyl-alanine ethyl ester is synthesized from the original real α-alanine, and is generally used under the catalysis of hydrochloric acid or hydrochloric acid-phosphoric acid. Realize the esterification of alanine, and then realize the oxalylation of amino group in the presence of deacidification agent, and its main reactio...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/10C07C235/80
Inventor 王祥忠
Owner CHANGSHU CHEM JIANGSU
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com