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Preparation method of pyridoxamine dihydrochloride

A technology of pyridoxamine dihydrochloride and pyridoxamine, which is applied in the field of preparation of pyridoxamine dihydrochloride, can solve the problems of large solvent consumption and high cost, reduce preparation cost, save organic raw materials and solvents Effect

Inactive Publication Date: 2010-01-20
SUZHOU FUSHILAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has problems such as high cost and large solvent consumption.

Method used

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  • Preparation method of pyridoxamine dihydrochloride
  • Preparation method of pyridoxamine dihydrochloride
  • Preparation method of pyridoxamine dihydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A) preparation of pyridoxine:

[0027] First add 100g (0.486mol) pyridoxine hydrochloride and 750g pure water in the 2000ml four-necked reaction flask equipped with stirring device and thermometer, stir at room temperature, pyridoxine hydrochloride is dissolved, then add active 75g (0.863mol) of manganese dioxide and 90g (0.918mol) of concentrated sulfuric acid were added dropwise, the reaction temperature was controlled at 40-45°C, and the time for adding the concentrated sulfuric acid was 45min. 48 DEG C of reaction, by TLC monitoring reaction, after the pyridoxine hydrochloride reaction as starting material is complete, obtain active substance pyridoxal, then add anhydrous sodium acetate 150g (1.83mol) and hydroxylamine hydrochloride 59.4g (0.855 mol) reaction, the reaction temperature is 55-60 ° C, reacted under stirring for 30 minutes, and finally through cold analysis, filtration and drying, 81.4 g of pyridoxine was obtained, the molar yield was 92%, and the chemi...

Embodiment 2

[0035] A) preparation of pyridoxine:

[0036] First add 50g (0.243mol) pyridoxine hydrochloride and 400g pure water in the 1000ml four-necked reaction flask equipped with stirring device and thermometer, stir at room temperature, pyridoxine hydrochloride is dissolved, then add active 37.5g (0.43mol) of manganese dioxide and 45g (0.46mol) of concentrated sulfuric acid were added dropwise, the reaction temperature was controlled at 40-45°C, and the time for adding concentrated sulfuric acid was 45min. -48 DEG C of reaction, by TLC monitoring reaction, treat after the pyridoxine hydrochloride reaction as starting material is complete, obtain active substance pyridoxal, then add anhydrous sodium acetate 75g (0.915mol) and hydroxylamine hydrochloride 29.7g ( .428mol) reaction, reaction temperature is 55-60 ℃, reacts 30min under stirring state, finally through cold analysis, filtration and drying, obtains pyridoxine 40.8g, and molar yield is 92%, and chemical purity is 99.5%. This ...

Embodiment 3

[0040] A) preparation of pyridoxine:

[0041] First add 120g (0.583mol) pyridoxine hydrochloride and 900g pure water in the 2000ml four-necked reaction flask that stirring device and thermometer are housed, stir at room temperature, pyridoxine hydrochloride is dissolved, then add active 90g (1.03mol) of manganese dioxide and 108g (1.1mol) of concentrated sulfuric acid were added dropwise, the reaction temperature was controlled at 40-45°C, and the time for adding the concentrated sulfuric acid was 45min. 48 DEG C of reaction, by TLC monitoring reaction, after the pyridoxine hydrochloride reaction as starting material is complete, obtain active substance pyridoxal, then add anhydrous sodium acetate 180g (2.2mol) and hydroxylamine hydrochloride 71.3g (1.03 mol) reaction, the reaction temperature is 55-60 ° C, and the reaction is carried out under stirring for 30 minutes, and finally through cold analysis, filtration and drying, 98.0 g of pyridoxine is obtained, the molar yield i...

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Abstract

The invention relates to a preparation method of pyridoxamine dihydrochloride, belonging to the technical field of the preparation of water soluble vitamins. The preparation method comprises the following steps: preparing pyridoxal oxime: taking pyridoxine hydrochloride as initial raw material and water as a reaction medium, adding activated manganese dioxide and concentrated sulfuric acid to generate pyridoxal by the reaction, and then reacting with anhydrous sodium acetate and hydroxylamine hydrochloride to obtain pyridoxal oxime; preparing pyridoxamine dihydrochloride: firstly enabling pyridoxal oxime to react with acetic acid and zinc to obtain acetic acid solution containing pyridoxamine, then decompressing the solution and reclaiming the acetic acid to obtain slurry concentrate, decompressing and reclaiming the acetic acid again to obtain pyridoxamine water solution, regulating the pH value to be alkaline so as to separate pyridoxamine out, adding water and hydrochloric acid after vacuum filteration, decoloring and filtering to obtain filtrate, decompressing and concentrating the filtrate until white solids are separated out, adding solvent and stirring, and finally crystallizing at the lower temperature, filtering and drying to obtain the pyridoxamine dihydrochloride. The invention has the advantages that the prepared pyridoxamine dihydrochloride has high total mol yield and purity, and the preparation method is reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of water-soluble vitamins, and in particular relates to a preparation method of pyridoxamine dihydrochloride. Background technique [0002] Pyridoxamine dihydrochloride is also known as vitamin B 6 Dihydrochloride is one of the water-soluble B vitamins. The chemical name of pyridoxamine dihydrochloride is: 2-methyl-3-hydroxyl-4-aminomethyl-5-hydroxymethylpyridine dihydrochloride; molecular formula is: C 8 h 12 N 2 o 2 ·2Hcl; molecular weight: 241.11; English name: Pyridoxamide Dihydrochloride. The structural formula of pyridoxamine dihydrochloride is as follows: [0003] [0004] Pyridoxamine is a vitamin B 6 One of the three natural forms of vitamin B, which has relatively little side effects on the human body. For a long time, various forms of vitamin B 6 It has been used as a food additive (also known as food supply) and medical treatment. In the treatment of various chronic dis...

Claims

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Application Information

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IPC IPC(8): C07D213/66
Inventor 陆建刚邢健
Owner SUZHOU FUSHILAI PHARMA CO LTD
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