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L-arginine alpha-ketoisocaproate preparation method

A technology of ketoisocaproic acid and isocaproate, which is applied in the field of preparation of L-arginine a-ketoisocaproate, can solve the problems of high total cost, inability to apply solvents, and high requirements for solvents and reaction systems. achieve good looseness

Inactive Publication Date: 2017-05-17
江西乐维生物药业有限公司
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  • Summary
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  • Claims
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AI Technical Summary

Problems solved by technology

[0007] The defect of this method is that because of the strong hygroscopicity of L-arginine α-ketoisocaproate, if there is a very small amount of water in the solvent or reaction system, well-solidified crystals cannot be obtained, and the material is extremely fluid. Poor jelly, so the requirements for the solvent and reaction system used are very high. In addition, because ethanol and a large amount of ethyl acetate are used, the filtrate after filtration is a mixture of ethanol and ethyl acetate, which needs to be diluted with a large amount of water. Dissolving ethanol into water to achieve the purpose of separation from ethyl acetate, the recovered solvent cannot be applied to the production of this product, and the total cost is very high.

Method used

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Embodiment Construction

[0014] Specific operation examples:

[0015] Reaction equation:

[0016]

[0017]

[0018] Equipment: Mechanical Stirrer S312-90

[0019] High Speed ​​Centrifugal Spray Dryer RY-LGP-5

[0020] Operation process:

[0021] Accurately weigh 100 grams of a-ketoisocaproic acid, put it into a 1000ml three-necked flask, add 600ml of water, heat to 60-70°C, then slowly add L-arginine in portions to adjust the solution system to neutral Finally, add 10 grams of activated carbon, stir at 60-70° C. for 1 hour, filter while hot, and collect the filtrate.

[0022] Turn on the heating of the high-speed centrifugal spray dryer in advance, set the air inlet temperature at 130-135°C, and when the temperature is constant, add the filtrate prepared earlier into the solution tank, and control the flow rate of the feed pump at 5-10ml / min, so that after The material after centrifugal spray drying is collected in granular form at the discharge port. 160 g of L-arginine a-ketoisocaproate w...

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Abstract

The invention relates to a L-arginine alpha-ketoisocaproate preparation method. The method comprises the following steps: accurately weighing 100 g of keto isocaproic acid, placing the material in a 1000 ml of flask, adding 600 ml of water, heating the material to the temperature of 60-70 DEG C, gradually adding L-arginine, adjusting a solution to neutrality, adding 10 g of active carbon, stirring the material for1 hour at the temperature of 60-70 DEG C, filtering the material while hot, collecting a filtrate; turning on a high-speed centrifuging and spraying drier for heating the material, setting the air intake temperature at 130-135 DEG C, adding the prepared filtrate in a solution pot, controlling the flow velocity of a charge pump at 5-10 ml / min, and collecting the material after centrifugal spray drying to a granular state at a discharge hatch, and obtaining the 160 g of white powder L-arginine alpha-ketoisocaproate. The method has the advantages of simple production step, and convenient and practical performances.

Description

technical field [0001] The invention relates to a preparation method of L-arginine α-ketoisocaproate. Background technique [0002] The structural formula of L-arginine a-ketoisocaproate is: [0003] [0004] Molecular formula: C 18 h 34 N 4 o 8 ; Molecular weight: 434.5; [0005] Properties: white crystalline powder. [0006] At present, the production method of this product in China is to mix a-ketoisocaproic acid and an appropriate amount of absolute ethanol, heat it to a suitable temperature, slowly add L-arginine, adjust to neutrality, and slowly dissolve the reaction solution. Add it to a large amount of anhydrous ethyl acetate at a suitable temperature. After strong and rapid stirring for a long time, the material gradually solidifies and crystallizes, and then cools down, filters and dries to obtain the finished product. [0007] The defect of this method is that because of the strong hygroscopicity of L-arginine α-ketoisocaproate, if there is a very small ...

Claims

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Application Information

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IPC IPC(8): C07C277/08C07C279/14C07C51/41C07C59/185
CPCC07C277/08C07C51/412C07C279/14C07C59/185
Inventor 林忠贵李江晖
Owner 江西乐维生物药业有限公司
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