Technique for preparing L-homoserine

A technology of homoserine and a new process, which is applied in the field of preparation of homoserine, can solve the problems of inflammability and explosion, technical level limitation, "three wastes" pollution, etc., and achieve the effect of increasing product yield, reducing production cost, and simplifying process steps

Inactive Publication Date: 2008-01-09
安徽省恒锐新技术开发有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its demand is increasing year by year, but due to the limitation of technical level, the production of this product has not been able to meet the demand
[0003] At present, the L-homoserine synthesis process route developed at home and abroad mainly includes the synthesis route using L-methionine as raw material. This route is due to the use of flammable, explosive and toxic raw materials, and the synthesis route is long and the product The post-processing is cumbersome, the pollution of "three wastes" is serious, and the overall benefit is poor

Method used

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  • Technique for preparing L-homoserine

Examples

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Effect test

Embodiment 1

[0022] Step 1 Preparation of L-Aspartic Acid Methyl Ester

[0023] Add 133.1g of L-aspartic acid (1.0mol) and 1000ml of anhydrous methanol into a 2000ml three-neck flask, and feed 73g of HCl at below 5°C. After passing through, the temperature was slowly raised to reflux for 2 hours, and the organic solvent was evaporated under reduced pressure to obtain 165.2 g of white crystal L-aspartic acid methyl ester hydrochloride, with a purity of 98.5% and a yield of 90.0% (using L-tianmen aspartic acid meter).

[0024] Step 2 Preparation of L-homoserine by reduction of L-aspartic acid methyl ester

[0025] Take the above 73.5g of L-aspartic acid methyl ester hydrochloride (0.4mol), add 1100g of anhydrous methanol into a 2000mL three-necked flask and mix evenly, and adjust the pH to 5 with triethylamine, then slowly add 31g (0.8mol )NaBH 4 , The feeding temperature is controlled at 0-5°C, and the adding speed of the reducing agent is controlled to prevent the reaction from being to...

Embodiment 2

[0027] Step 1 Preparation of L-ethyl aspartate

[0028] Add 133.1g of L-aspartic acid (1.0mol) and 1000ml of absolute ethanol into a 2000ml three-necked flask, and feed 73g of HCl at below 5°C. After passing through, the temperature was slowly raised to reflux for 2 hours, and the organic solvent was evaporated under reduced pressure to obtain 180.0 g of white crystal L-aspartic acid ethyl ester hydrochloride with a purity of 98.6% and a yield of 91.1% (using L-tianmen aspartic acid meter).

[0029] Step 2 Preparation of L-homoserine by reduction of L-aspartic acid ethyl ester

[0030] Take the above 79.0g of L-aspartic acid ethyl ester hydrochloride (0.4mol), add 790g of absolute ethanol into a 1500mL three-necked flask and mix evenly, and adjust the pH to 5 with triethylamine, then slowly add 31g (0.8mol )NaBH 4 , The feeding temperature is controlled at 0-5°C, and the adding speed of the reducing agent is controlled to prevent the reaction from being too violent or the l...

Embodiment 3

[0032] Step 1 Preparation of L-Aspartic Acid Methyl Ester

[0033] Add 133.1g of L-aspartic acid (1.0mol) and 1000ml of anhydrous methanol into a 2000ml three-neck flask, and feed 73g of HCl at below 5°C. After passing through, the temperature was slowly raised to reflux for 2 hours, and the organic solvent was evaporated under reduced pressure to obtain 165.2 g of white crystal L-aspartic acid methyl ester hydrochloride, with a purity of 98.5% and a yield of 90.0% (using L-tianmen aspartic acid meter).

[0034] Step 2 Preparation of L-homoserine by reduction of L-aspartic acid methyl ester

[0035] Take the above 73.5g L-aspartic acid methyl ester hydrochloride (0.4mol), add 750g of anhydrous methanol into a 1500mL three-necked flask and mix evenly, and adjust the pH to 5 with triethylamine, then slowly add 18.5g (0.48 mol)LiAlH 4 , The feeding temperature is controlled at 0-5°C, and the adding speed of the reducing agent is controlled to prevent the reaction from being to...

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Abstract

Production of L-homoserine is carried out by taking L-asparto as raw material to prepare L-asparto methyl ester or ethyl ester, taking them as raw materials, taking metal complex hydrogen compound as reducer, and preparing final product under normal pressure in organic solvent. It's convenient, has gentle reactive condition and can be used for industrial production.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and relates to a new process for preparing L-homoserine, especially a new process for preparing homoserine with L-aspartic acid as a raw material, which belongs to the reduction reaction technology for preparing L-homoserine field. Background technique [0002] L-homoserine (chemical name: 2-amino-4-hydroxybutyric acid) is a pharmaceutical intermediate and the main raw material for the synthesis of L-glufosinate. Glufosinate is a systemic conduction herbicide with broad-spectrum herbicidal activity. L-Glufosinate has been widely used in developed countries because of its high herbicidal activity. Its demand is increasing year by year, but due to the limitation of technical level, the production of this product has not been able to meet the demand. [0003] At present, the L-homoserine synthesis process route developed at home and abroad mainly includes the synthesis route using L-m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/22C07C227/14
Inventor 马云峰王祖元吴梅
Owner 安徽省恒锐新技术开发有限责任公司
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