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A kind of preparation method of metadoxine impurity compound

A technology of metadoxine and compounds, which is applied in the field of preparation of metadoxine impurity compounds, can solve problems such as hidden dangers of drug quality, impact on health, and rare preparation methods, and achieve the effect of improving quality standards

Active Publication Date: 2018-03-09
SICHUAN TONGSHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, existing studies have shown that there are some specific impurities in metadoxine medicines, which are a major hidden danger to the quality of medicines and seriously affect the health of people who use metadoxine medicines
At present, there are no relevant reports on the research and disclosure of these specific impurities, and their preparation methods are even rarer, which has brought many problems to people in the process of improving the quality of metadoxine drugs.

Method used

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  • A kind of preparation method of metadoxine impurity compound
  • A kind of preparation method of metadoxine impurity compound
  • A kind of preparation method of metadoxine impurity compound

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Under the protection of nitrogen, add 50g of metadoxine and 500ml of water into a 1L pressure reactor; start stirring, and adjust the pH of the reaction system to 6.0 with 20% aqueous sodium hydroxide solution after the solid is dissolved, and control the reaction temperature to 50°C and the reaction pressure 9.5 psi, reaction 3 hours. TLC monitors until the reaction is complete. The reaction solution was concentrated under reduced pressure and purified by column chromatography to obtain a solid, namely metadoxine impurity compound, with a weight of 5.7 g, a yield of 21.9%, and a purity of 98.8%. NMR (in D 2 (O is solvent) and after high-resolution mass spectrometry detection, the structural formula of this metadoxine impurity compound is Its molecular formula is C 16 h 21 N 2 o 5 , whose chemical name is 1-((3-hydroxy-5-(hydroxymethyl)-2-methylpyridin-4-yl)methyl)-4,5-bis(hydroxymethyl)-2-methyl Pyridin-1-ium-3-ol inner salt.

[0029] The following are proton ...

Embodiment 2

[0035] Under nitrogen protection, add 50g of metadoxine, 300ml of methanol and 100ml of water into a 1L pressure reactor; start stirring, and adjust the pH of the reaction system to 6.0 with 20% aqueous sodium hydroxide solution after the solid is dissolved, and control the reaction temperature to 50°C , pressure is 9.5psi, reacts for 3 hours, TLC monitors until the reaction is complete; the reaction solution is concentrated under reduced pressure, and purified by column chromatography to obtain a solid, namely metadoxine impurity compound, with a weight of 9.9g, a yield of 38.1%, a purity of was 98.7%. Other measures are with embodiment 1.

Embodiment 3

[0037] Under nitrogen protection, add 50g metadoxine, 300ml isopropanol and 100ml water in a 1L pressure reactor; start stirring, adjust the pH of the reaction system to 6.0 with 20% aqueous sodium hydroxide solution after the solid is dissolved, and control the reaction temperature to 50°C, reaction pressure 5psi, reacted for 3 hours; TLC monitored until the reaction was complete, the reaction solution was concentrated under reduced pressure, and purified by column chromatography to obtain a solid, namely metadoxine impurity compound, with a weight of 11.2g and a yield of 43.2%. , with a purity of 98.5%. Other measures are with embodiment 1.

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Abstract

The invention discloses a method for preparing a metadoxine impurity compound. Metadoxine is dissolved in a water-containing solvent, the pH value of a reaction system is adjusted to be 5.0-8.0 with an alkaline reagent, the reaction temperature is controlled to be 30-100 DEG C, the reaction pressure is controlled to be 0-33 psi, reaction lasts for 3-8 hours, the metadoxine impurity compound is obtained, and the metadoxine impurity compound is purified through column chromatography. The purity of metadoxine impurities prepared through the method can reach 98.8%, and the metadoxine impurities can serve as a reference substance and be used for quality research. The metadoxine impurity compound is obtained so that improvement of the quality standard of metadoxine medicine can be promoted, and a health guarantee is provided for people to use the metadoxine medicine.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a method for preparing metadoxine impurity compounds. Background technique [0002] At present, Metadoxine, whose chemical name is pyridoxine L-2 pyrrolidone-5-carboxylate, was developed by the Italian Laboratori Baldacci SPA company and was launched in Italy in September 1985 under the trade name Metadoxil; its indication is alcohol Sexual liver disease. The population of patients with alcoholic liver disease is huge and has a growing trend. As a drug for the treatment of alcoholic liver disease, metadoxine can improve liver function damage caused by long-term drinking. Animal experiments have shown that metadoxine has the effect of anti-lipid peroxidation of liver cells, and can reduce the accumulation of fat in liver cells of animals with chronic alcoholism; Alcohol dehydrogenase (ADH) is converted into acetaldehyde, acetaldehyde is converted into acetic acid by acetaldehyde dehydro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/66
CPCC07D213/66
Inventor 黄青春黄春蒋雨竹李大萍李丽川黄婷
Owner SICHUAN TONGSHENG BIOTECH
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