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Preparation method of alpha-ketophenylalanine calcium

A technology of calcium ketophenylalanine and purification method, which is applied in the preparation of carboxylate, the preparation of carboxylate, the preparation of organic compounds, etc., can solve the problems of low utilization rate of equipment, complicated operation, and high initial investment cost, and achieves The effect of reducing environmental pressure, high safety factor, and uniform API particle size

Active Publication Date: 2021-10-01
BEIJING WINSUNNY PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this preparation method, methods and equipment such as decolorization and filtration, freezing crystallization, and partition membrane filter press are used, and the operation is complicated, the utilization rate of the equipment is low, and the initial investment cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Preparation of α-ketophenylalanine calcium

[0038] a) Add 1750g of water, 350g (3.47mol) of hydantoin to a 10L four-necked flask, then add 393g (3.70mol) of benzaldehyde (3.70mol) and 194g (2.62mol) of calcium hydroxide into the reaction flask in turn, raise the temperature to 20°C, and keep warm React for 2 hours to obtain a reaction solution containing benzylidene hydantoin (containing undissolved calcium hydroxide solid);

[0039] b) The above reaction solution (containing undissolved calcium hydroxide solid) is heated to 100°C, heated to reflux, and reacted for 5 hours to obtain a solution containing calcium α-ketophenylalanine;

[0040] c) Cool the above-mentioned solution containing α-ketophenylalanine calcium to 40°C, control the temperature at 40°C, slowly add 31% hydrochloric acid dropwise to adjust the pH to 6.5, control the temperature at 40°C and keep it for 2 hours, then cool it down to 20°C, keep it warm Crystallize for 2 hours, filter with suction, an...

Embodiment 2

[0044] (1) Preparation of α-ketophenylalanine calcium

[0045] a) Add 1750g of water, 350g (3.47mol) of hydantoin to a 10L four-necked bottle, then add 423g (4.00mol) of benzaldehyde (4.00mol) and 257g (2.47mol) of calcium hydroxide into the reaction flask in turn, raise the temperature to 30°C, and keep warm React for 2 hours to obtain a reaction solution containing benzylidene hydantoin (containing undissolved calcium hydroxide solid);

[0046] b) The above reaction solution (containing undissolved calcium hydroxide solid) is heated to 100°C, heated to reflux, and reacted for 4 hours to obtain a solution containing calcium α-ketophenylalanine;

[0047] c) Cool the above-mentioned solution containing α-ketophenylalanine calcium to 45°C, control the temperature at 45°C, slowly add 31% hydrochloric acid dropwise to adjust the pH to 7, control the temperature at 45°C and keep it for 2 hours, then cool it down to 10°C, keep it warm Crystallize for 2 hours, filter with suction, a...

Embodiment 3

[0051] (1) Preparation of α-ketophenylalanine calcium

[0052] a) Add 1750g of water, 350g (3.47mol) of hydantoin to a 10L four-necked bottle, then add 405g (3.82mol) of benzaldehyde (3.82mol) and 180g (2.43mol) of calcium hydroxide into the reaction flask in turn, raise the temperature to 25°C, and keep warm React for 2 hours to obtain a reaction solution containing benzylidene hydantoin (containing undissolved calcium hydroxide solid);

[0053] b) The above-mentioned reaction solution (containing undissolved calcium hydroxide solid) is heated to 95°C, heated to reflux, and reacted for 4 hours to obtain a solution containing calcium α-ketophenylalanine;

[0054] c) Cool the above-mentioned solution containing α-ketophenylalanine calcium to 40°C, control the temperature at 40°C, slowly add 31% hydrochloric acid dropwise to adjust the pH to 7.5, control the temperature at 40°C and keep it for 2 hours, then cool it down to 10°C, keep it warm Crystallize for 2 hours, filter with...

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Abstract

The invention relates to a preparation method of alpha-ketophenylalanine calcium and a purification method of the alpha-ketophenylalanine calcium. The preparation method comprises the following steps: reacting hydantoin, benzaldehyde and calcium hydroxide in water to obtain a reaction system containing benzylidene hydantoin; heating the reaction system for hydrolysis reaction to obtain an alpha-ketophenylalanine calcium solution; and adjusting the pH value of the alpha-ketophenylalanine calcium solution to 5-8, and crystallizing to obtain the alpha-ketophenylalanine calcium. The method is green, environment-friendly, few in generated three wastes, few in operation steps, simple and easy to implement; and meanwhile, the alpha-ketophenylalanine calcium prepared by the method has relatively high yield and purity.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of alpha-ketophenylalanine calcium and a further purification method of alpha-ketophenylalanine calcium. Background technique [0002] α-ketophenylalanine is the precursor of the biosynthesis of essential amino acid phenylalanine, and is an important raw material of compound α-ketoacid tablets. α-Ketophenylalanine and its salts are also important ingredients in energy drinks. Compound α-ketoacid tablets can increase glomerular filtration and urinary albumin excretion, and it can reduce the symptoms of uremia patients with a low-protein diet, and has played a good role in slowing down the deterioration of renal function. [0003] According to literature reports, the synthesis of α-ketophenylalanine calcium mainly has the following three methods: Route 1 uses 1-phenyl-2-propanone as raw material, and generates α-ketophenylalanine through oxidati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/00C07C51/43C07C59/84
CPCC07C51/41C07C51/43C07C59/84
Inventor 刘志东霍玉魁李志刚吕振远宋立起
Owner BEIJING WINSUNNY PHARMA CO LTD
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