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Cleaning production method of raw drug N-trimethyl lysine and application method

A technology of trimethyl lysine and a production method is applied in the field of clean production and application of raw material drug-N-trimethyl lysine, and can solve the problems of difficulty in guaranteeing the quality of laminine, pollution of factory areas and environment, etc. , to eliminate the danger of polluting the production workshop and the environment, achieve good quality, and achieve the effect of cleaner production

Inactive Publication Date: 2006-01-25
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, in the existing technology, the Chinese patent application CN 97123269.5 discloses a preparation method of laminin, but toxic copper carbonate, dimethyl sulfate and hydrogen sulfide are used as raw materials in the synthesis process, which is not only difficult to ensure that it can be used as a medicine The quality of laminin, but also cause defects such as factory area and environmental pollution

Method used

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  • Cleaning production method of raw drug N-trimethyl lysine and application method
  • Cleaning production method of raw drug N-trimethyl lysine and application method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] In the 500L reaction kettle, first add 300 kg of distilled water, weigh 75 kg of food grade (feed grade) zinc sulfate and stir for 20 minutes to dissolve, and then slowly add 91 kg of L-lysine hydrochloride to the reaction kettle under stirring , 60 ℃ constant temperature reaction for 1 hour, let lysine and Zn 2+ The reaction is complete; then react with 135 kilograms of dimethyl carbonate to generate the complex of quaternized lysine derivative, then with 79 kilograms of ethylenediaminetetraacetic acid disodium salt, metal ion unmasking reaction occurs to obtain N-trimethyl The crude lysine product was finally adsorbed N-trimethyl lysine using a strong acid cation resin exchange column, washed with deionized water or ethanol, concentrated under negative pressure, and crystallized to obtain 110 kilograms of raw material N-trimethyl lysine. .

Embodiment 2

[0031] In a 100L reaction kettle, first add 55 kg of distilled water, weigh 13 kg of drinking-grade ferrous sulfate and stir for 20 minutes to dissolve, and then slowly add 19 kg of L-lysine hydrochloride to the reaction kettle under stirring, at 60° C. Constant temperature reaction for 1 hour, let lysine and Fe 2+ The reaction is complete; Then react with 27 kilograms of dimethyl carbonate to generate the complex of quaternized lysine derivative, then with 16 kilograms of ethylenediaminetetraacetic acid disodium salts, the metal ion unmasking reaction occurs to obtain the laminarin crude product, Finally, a strong acid cation resin exchange column was used to adsorb N-trimethyllysine, and 21 kg of raw material N-trimethyllysine was obtained by washing and purifying with deionized water, desorption with dilute ammonia water, vacuum concentration and crystallization.

Embodiment 3

[0033] In a 200L reaction kettle, first add 100 kg of distilled water, weigh 27 kg of feed-grade copper sulfate and stir for 20 minutes to dissolve, then slowly add 37 kg of L-lysine hydrochloride to the reaction kettle under stirring, and keep it at a constant temperature of 60°C. React for 1 hour to allow lysine to react with Cu 2+ The reaction is complete; Then react with 54 kilograms of dimethyl carbonate to generate the complex of quaternized lysine derivative, then with 31 kilograms of ethylenediaminetetraacetic acid disodium salts, the metal ion unmasking reaction takes place to obtain the laminarin crude product, Finally, a strong acid cation resin exchange column is used to adsorb N-trimethyllysine, and 40 kg of raw material N-trimethyllysine is obtained through deionized water washing and purification, dilute ammonia desorption, vacuum concentration and crystallization.

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Abstract

The invention discloses a method for the clean production of N-trimethyllysine and method of application, wherein the production method consists of screening and protecting alpha-amino with metallic ions, carrying out epsilon-amino reaction between dimethyl carbonate, an environment-friendly type methylating reagent with lysine, obtaining quaternized lysine derivative (N-trimethyllysine metallic complex), finally de-screening the metallic ions with amino carboxyl chelating agent, then isolating and purifying with ion exchange process so as to obtain medicinal grade of N-trimethyllysine, which can be used as the raw material for medicament for preventing or treating high blood pressure, lowering blood fat, maintaining blood vessel, or as food, health product additives.

Description

Technical field: [0001] The invention relates to a clean production method of laminine, in particular using non-toxic and environment-friendly chemical raw materials and modern ion exchange technology in the whole preparation process of N-trimethyl lysine, which not only ensures the N-trimethyl lysine The quality requirements of base lysine as a pharmaceutical or food additive, at the same time, it truly ensures that N-trimethyl lysine is a green product. N-trimethyllysine can be used not only as an API for preventing cardiovascular and cerebrovascular diseases, but also as an additive for food and health care products. Background technique: [0002] Kelp is a well-known edible algae that is rich in nutrients. Kelp contains a non-protein amino acid with special physiological function, namely N-trimethyl lysine. Because kelp is another name for kelp, N-trimethyl lysine is also called laminine. N-trimethyllysine has a special blood pressure lowering effect, which can prevent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/26C07C227/18
Inventor 李群李子超李艳春
Owner QINGDAO UNIV
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