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Method for purifying L-valine from L-valine complex

A valine and compound technology, applied in the field of purifying L-valine, can solve the problems of many impurities affecting the purity and quality of finished products, and achieve the effects of high purification yield, low cost and low pollution

Active Publication Date: 2017-12-19
HUANGGANG WELLMAN BIOSCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Purification of L-valine prior art at present is to use physical method and ion exchange process to obtain finished product through decolorization, concentration and crystallization etc. purification of L-valine crude product in fermented liquid, in the L-valine of this method purification usually Contains alanine, leucine, isoleucine, etc. with similar chemical properties, and there are many impurities, which affect the purity and quality of the finished product

Method used

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  • Method for purifying L-valine from L-valine complex
  • Method for purifying L-valine from L-valine complex
  • Method for purifying L-valine from L-valine complex

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 1000ml reaction bottle, add 100g of L-valine complex, add 300g of methanol, stir and heat up to reflux for 60min, filter while hot, return the solid to the kettle, continue to add 300g of methanol, stir and heat up to reflux for 60min, filter while hot, repeat this three times , dried to obtain 33g of L-valine crude product, dissolved the solid in 350ml of water, added 0.3g of activated carbon, boiled and decolorized for 45min, filtered while hot, concentrated the filtrate to 100ml under reduced pressure, and L-valine solid precipitated, cooled to 25 °C filtration to obtain 25 g of L-valine.

Embodiment 2

[0027] 1000ml reaction bottle, add 100g of L-valine complex, add 250g of ethanol, stir and raise the temperature to reflux for 60min, filter while hot, return the solid to the kettle, continue to add 250g methanol, stir and raise the temperature to reflux for 60min, filter while hot, repeat this three times , and dried to obtain 35.5 g of L-valine crude product. Dissolve the solid in 400ml of water, add 0.4g of activated carbon, boil for 30min to decolorize, filter while hot, concentrate the filtrate to 100ml under reduced pressure, L-valine solid precipitates, cool to 30°C and filter to obtain 30g of L-valine.

Embodiment 3

[0029] 1000ml reaction bottle, add 150g of L-valine complex, add 440g of methanol, stir and raise the temperature to reflux for 2h, filter while hot, return the solid to the kettle, continue to add 440g of methanol, stir and raise the temperature to reflux for 2h, filter while hot, repeat this three times , and dried to obtain 52 g of L-valine crude product. Dissolve the solid in 600ml of water, add 0.50g of activated carbon, boil for 45min to decolorize, filter while hot, concentrate the filtrate to 100ml under reduced pressure, L-valine solid precipitates, cool to 25°C and filter to obtain 42g of L-valine.

[0030] Evidence of the positive (beneficial) effects that can be produced by applying the present invention

[0031] Table 1 embodiment 1 product quality standard and technical index

[0032]

[0033] Table 2 embodiment 2 product quality standards and technical indicators

[0034]

[0035]

[0036] Table 3 embodiment 3 product quality standards and technical i...

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Abstract

The present invention relates to a method for purifying L-valine from a L-valine complex. The method comprises: A, complexing racemic DL-valine and a resolving agent N-benzoyl-L-alanine to obtain an L-valine complex, adding 0.5-5 times the organic solvent to the L-valine complex, and carrying out heating reflux for 1-3 h in a reaction kettle; B, filtering the mixture obtained in the step A while hot, returning the solid to the kettle, adding 0.5-5 times the organic solvent, carrying out stirring reflux for 1-3 h, repeatedly performing three times, and filtering to obtain an L-valine crude product; C, adding 10-20 times the water to the crude product obtained in the step B, carrying out heating dissolving, decolorizing with active carbon, and filtering to obtain a decolorizing liquid; and D, carrying out pressure reducing concentration crystallization on the decolorizing liquid obtained in the step C in a crystallization kettle, filtering, and drying the wet product to obtain the L-valine finished product. According to the present invention, the hetero amino acids are not generated, the purification yield is obviously improved, the finished product quality is improved, the decolorizing liquid separation with the adsorption column in the traditional purification method is eliminated, and the operation is simple.

Description

technical field [0001] The invention relates to a method for purifying L-valine, in particular to a method for purifying L-valine from an L-valine compound. Background technique [0002] L-valine is an essential amino acid for the human body, which can maintain the normal functioning of the nervous system, enhance immunity, and promote liver regeneration. When the human body lacks L-valine, it is easy to cause growth stagnation and movement disorders. When the human body is seriously deficient, it will affect the growth and development of the body, causing neurological disorders, movement disorders, and anemia. As a nutritional supplement, it can be used together with other essential amino acids to prepare amino acid infusions and comprehensive amino acid preparations. L-valine is the key starting material for the preparation of valsartan, valganciclovir, ritonavir and lopinavir. Oxidants, etc., so L-valine has great utilization value in industries such as medicine and fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/34C07C227/40C07C227/42C07C229/08C07B57/00
CPCC07B57/00C07B2200/07C07C227/34C07C227/40C07C227/42C07C229/08
Inventor 熊绪杰胡松洲桂峰赵阳马丽
Owner HUANGGANG WELLMAN BIOSCI
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