Preparation method of crystal L-arginine alpha-ketoglutarate

A technology of ketoglutarate and ketoglutarate, applied in the field of amino acid salts, can solve the problems of complex L-arginine α-ketoglutarate, unsuitable for industrial production, poor crystal form, etc. Not easy to agglomerate, easy to transport and use, simple step effect

Inactive Publication Date: 2009-12-02
上海汉飞生化科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the preparation method of L-arginine α-ketoglutarate is complex in operation and low in yield, which is not suitable for industrial production and cannot meet the growing demand. At the same time, the product still has low purity and poor crystal form. shortcoming

Method used

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  • Preparation method of crystal L-arginine alpha-ketoglutarate

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Experimental program
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Effect test

Embodiment 1

[0025] A preparation method of crystalline L-arginine α-ketoglutarate: in a 500ml reaction bottle, add 70ml (69.6g) of 25% (weight) L-arginine solution (equivalent to 0.1molL - arginine), stirring, slowly add 14.6g (0.1mol) α-ketoglutaric acid, react at room temperature for 10mins, dissolve completely, then concentrate under reduced pressure, water bath temperature 55°C, concentrate the total volume of the reaction solution to about 56ml, cool to 23°C, slowly add 95% ethanol dropwise while stirring until a small amount of crystals are precipitated, stir for 10mins, then continue to add 95% ethanol dropwise, the total amount of ethanol is 42ml, and the dropping time is 2hr, then reduce the temperature of the crystallization solution to 5~10 ℃, stand for 30mins, make the crystal crystallize completely, filter, crystal wash with 95% ethanol, and vacuum-dry at 60 ℃, obtain white flaky crystal form L-arginine α-ketoglutarate (1: 1) 26.0g, the yield is 81.4%, the purity is 99.8%, [α...

Embodiment 2

[0027] A preparation method of crystalline L-arginine α-ketoglutarate: in a 500ml reaction bottle, add 70ml (69.6g) of 20% (weight) L-arginine solution (equivalent to 0.08molL - arginine), stir, slowly add 5.84g (0.04mol) α-ketoglutaric acid, react at room temperature for 10mins, dissolve completely, then concentrate under reduced pressure, water bath temperature 50°C, concentrate the total volume of the reaction solution to about 28ml, cool to 20°C, slowly add anhydrous methanol dropwise while stirring until a small amount of crystals are precipitated, stir for 10mins, then continue to add anhydrous methanol dropwise, the total amount of methanol is 168ml, and the dropping time is 2.5hr, then lower the temperature of the crystallization solution to 5-10°C, stand for 30mins, crystallize completely, filter, wash the crystals with anhydrous methanol, and vacuum-dry at 50°C to obtain white flaky crystals of L-arginine α-ketoglutarate (2 : 1) 15.89g, the yield is 80.4%, and the pu...

Embodiment 3

[0029] A preparation method of crystalline L-arginine α-ketoglutarate: in a 500ml reaction bottle, add 70ml (69.6g) of 30% (weight) L-arginine solution (equivalent to 0.12molL - arginine), stirring, slowly add 17.52g (0.12mol) α-ketoglutaric acid, react at room temperature for 10mins, completely dissolve, then concentrate under reduced pressure, water bath temperature 80°C, concentrate the total volume of the reaction solution to about 49ml, cool to 22°C, slowly add isobutanol dropwise while stirring until a small amount of crystals precipitate, stir for 10mins, and then continue to add isobutanol dropwise, the total amount of isobutanol is 63ml, and the dropping time is 2hr, and then the crystallization solution temperature Decrease to 5~10 ℃, stand 30mins, make crystal crystallize completely, filter, crystal wash with isobutanol, and vacuum-dry at 70 ℃, obtain white flaky crystalline L-arginine α-ketoglutarate ( 1:1) 26.5g, yield 82.8%, purity 98.6%, [α] D +16.0° (c=4, 6N H...

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Abstract

The invention relates to a preparation method of crystal L-arginine alpha-ketoglutarate, comprising the following steps: preparing water solution of L-arginine, and slowly adding alpha-ketoglutaric acid into the water solution, wherein the mol ratio of L-arginine and alpha-ketoglutaric acid is 1:1 or 2:1; reducing pressure and concentrating the alpha-ketoglutaric acid at 50-80 DEG C after complete dissolution, removing water accounting for 20-60 percent of the total volume and cooling to 20-30 DEG C; slowly adding an organic hydrophilic solvent or a mixed solvent of a polar hydrophilic solvent and a non-polar hydrophilic solvent; and carrying out temperature reduction, crystallization, filtering, washing and vacuum drying to obtain the crystal L-arginine alpha-ketoglutarate. Compared with the prior art, the invention has the advantages of reasonable process, simple steps, easy operation, good crystal form of the obtained product, difficult caking, convenient transportation and use, high purity (more than or equal to 98 percent) and high yield (80-86 percent) of the product, and the like, and is suitable for industrialization production.

Description

technical field [0001] The invention relates to amino acid salts, in particular to a preparation method of crystalline L-arginine α-ketoglutarate. Background technique [0002] L-arginine α-ketoglutarate is an amino acid salt health product with increasing sales in the international market. It is mainly used to improve human protein and enhance human physique. With the growing demand in the international market, the research on the crystallization method of L-arginine salt has become the focus of people's attention, especially the research on the method of salt-forming crystallization of L-arginine α-ketoglutarate Research. [0003] At present, the preparation method of L-arginine α-ketoglutarate is complex in operation and low in yield, which is not suitable for industrial production and cannot meet the growing demand. At the same time, the product still has low purity and poor crystal form. shortcoming. Contents of the invention [0004] The object of the present inve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/14C07C59/347A23L1/305A23L33/175
Inventor 苏建勇郑南华张建宇
Owner 上海汉飞生化科技有限公司
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