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Method for producing DL-homocysteine lactone hydrochlorate

A technology of cystine lactone and production method, which is applied in the field of production of DL-homocysteine ​​lactone hydrochloride, can solve the problems of high content of metal ion impurities, difficulty in reaching medical standards, and no disclosure of production methods, etc. problems, to achieve the effect of good quality, excellent quality and enhanced market competitiveness

Inactive Publication Date: 2008-03-19
湖北新生源生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product produced by this method has a high content of metal ion impurities, which is difficult to reach the medical standard
With this method, the product yield is generally 15%, and because the DL-homocystine product is used as a raw material, there is also the problem of high production cost
Therefore, the existing domestic DL-homocysteine ​​lactone hydrochloride product has weak market competitiveness and is a meager profit product
In addition, the production method described not only produces a large amount of hydrogen gas during the reaction, which is dangerous to operate, but also produces a large amount of waste water containing zinc or tin. If it is not properly treated, it will pollute the environment
According to literature reports, DL-homocysteine ​​lactone hydrochloride produced in foreign advanced countries is of good quality and can be directly used for the preparation of medicines. The yield is generally 18%, but its production method has not been disclosed.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Put 300kg DL-methionine and 600kg concentrated sulfuric acid in the reaction kettle, hydrolyze and reflux at a constant temperature of 100°C for 8 hours, after the hydrolysis, neutralize the hydrolyzate to pH=6 with concentrated ammonia water, cool and crystallize, and generate DL-homocystamine Acid crude product, filter and separate the crude product to obtain 328kg of crude product, dissolve the crude product in 5% dilute hydrochloric acid until completely dissolved, obtain 800L solution, add 5kg activated carbon for decolorization for 30 minutes, filter, the filtrate is electrolyzed with an ion diaphragm electrolyzer, and the anolyte With 5% dilute sulfuric acid, the cathode of the electrolytic plate is a platinum plate, the anode is an iridium plate, the electrolysis current is 280A, the voltage is 5V, and the electrolysis time is 14 hours. It is detected that there is no DL-homocystine in the catholyte, and then the crystallized catholyte is concentrated. The obtain...

Embodiment 2

[0022] Put 300kg DL-methionine and 600kg concentrated sulfuric acid in a reaction kettle, hydrolyze and reflux at a constant temperature of 140°C for 12 hours, after the hydrolysis is completed, neutralize the hydrolyzate to pH=4 with 40% sodium hydroxide solution, cool and crystallize, and generate DL - Homocystine crude product, filter and separate the crude product to obtain 335kg of the crude product, dissolve the crude product in 7% dilute hydrochloric acid until completely dissolved, obtain 800L solution, add 5kg of active carbon for decolorization for 30 minutes, filter, and use the filtrate with an ion-diaphragm electrolyzer Electrolysis, the anolyte uses 3% dilute nitric acid, the cathode of the electrolytic plate is a silver plate, the anode is a titanium-based composite plate, the electrolysis current is 280A, the voltage is 5V, the electrolysis time is 12 hours, and there is no DL-homocysteine ​​in the catholyte. Then concentrate the crystallization catholyte, filte...

Embodiment 3

[0024] Put 300kg DL-methionine and 600kg concentrated sulfuric acid in a reaction kettle, hydrolyze and reflux at a constant temperature of 120°C for 13 hours, after the hydrolysis is completed, neutralize the hydrolyzate to pH=3 with sodium bicarbonate, cool and crystallize, and separate the crude product by filtration. Obtain crude product 335kg, this crude product is dissolved in 9% dilute hydrochloric acid to dissolving completely, obtains 800L solution, adds 5kg gac to decolorize 30 minutes, filters, and the filtrate of clearing is electrolyzed with ionic membrane electrolyzer for filtrate, anolyte is diluted with 5% Sulfuric acid, the cathode of the electrolytic plate is a platinum plate, the anode is an iridium plate, the electrolysis current is 280A, the voltage is 5V, and the electrolysis time is 12 hours. It is detected that the catholyte has no DL-homocystine, and then the crystallized catholyte is concentrated, and the obtained DL—homocysteine ​​lactone hydrochlorid...

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Abstract

The present invention relates to a production method for DL-homocysteine lactone hydrochloride. The present invention adopts DL-methionine as the raw material, obtains DL-homocystine through the catalyzing and the hysrolyzing of concentrated sulfuric acid at a certain temperature and time, and electrolyzes the crystal of the obtained substance in chlorhydric acid medium to get the product. The present invention can realize that the content of the product is up to 99.8 percent-101.5 percent, the purity is over 99.5 percent, the yield is about 30 percent, and no water is discharged during the production process.

Description

technical field [0001] The present invention relates to the production method of DL-homocysteine ​​lactone hydrochloride. Background technique [0002] DL-homocysteine ​​lactone hydrochloride, the product form is white crystalline powder. It is an important biochemical agent and drug intermediate, which can be used to prepare MR-2407, Citilone and other drugs. [0003] In the prior art, the domestic production of DL-homocysteine ​​lactone hydrochloride widely uses the method of obtaining the product through the action of the reducing agent zinc or tin and hydrochloric acid on the raw material DL-homocysteine. The product produced by this method has a high content of metal ion impurities, which is difficult to reach the medical standard. With this method, the product yield is generally 15%. Since the DL-homocystine product is used as a raw material, there is still the problem of high production cost. Therefore, the existing domestic DL-homocysteine ​​lactone hydrochloride ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00C07D309/30
Inventor 章平吕启超高艺娥徐建华
Owner 湖北新生源生物工程有限公司
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