Preparation method of alpha-ketophenylalanine calcium

Abstract

The invention discloses an alpha-ketophenylalanine calcium preparation method. The alpha-ketophenylalanine calcium preparation method comprises the following steps of: mixing glycolylurea, medium strong base and water, adding benzaldehyde, reacting to separate out isobutylidene glycolylurea, dropwise adding strong base liquor, stirring and heating till reflowing, reacting, adjusting the pH, extracting, adding alkali to an organic phase, uniformly mixing, adding water for extraction, adding alcohol to a water phase, dropwise adding a calcium chloride aqueous solution for heat preservation and reaction, filtering and washing to prepare the alpha-ketophenylalanine calcium. According to the alpha-ketophenylalanine calcium preparation method, after condensation reaction is ended, the isobutylidene glycolylurea is not separated and directly hydrolyzed, the utilization rate of equipment can be increased by 30%, the operation is simple, extracted alpha-ketophenylalanine does not need to be concentrated, the decomposition of the alpha-ketophenylalanine can be avoided during concentration, the alpha-ketophenylalanine is directly converted into ammonium salt in the organic phase, and then the ammonium salt is converted into calcium salt in the water phase, reaction conditions are mild, the purity is high, the total impurity is less than or equal to 5%, the cost is low, few wastewater is generated, the pollution to the environment is little, the raw materials are easy to obtain, the product quality is stable, the reaction yield of the method is 10% higher than that of the prior art, qualified products are directly obtained through salt forming reaction, and the multiple recrystallizaiton is avoided; and the alpha-ketophenylalanine calcium preparation method has no special requirements on equipment and is suitable for industrial production.

Description

technical field [0001] The invention relates to pharmaceutical and chemical intermediates, in particular to a preparation method of α-ketophenylalanine calcium. technical background [0002] α-ketophenylalanine is the precursor of the biosynthesis of phenylalanine, an essential amino acid for the human body, and is an important raw material for compound α-ketoacid products. In functional beverages, α-ketophenylalanine and its salts are also important ingredients. As one of the normal metabolites of the human body, α-keto acid can also be directly used in the treatment of some uremia. At present, compound α-keto acid preparation combined with low-protein diet therapy can reduce the symptoms of uremia patients and slow down the renal function. Functional deterioration has played a good role. Compound α-keto acid was developed and marketed by Fresenius Kabi, Germany. Compound α-ketoacid tablets can improve renal function, blood lipid disorder and nutritional status of patien...

AI Technical Summary

Problems solved by technology

Comparing the above three methods, it is found that the raw materials of synthetic routes 1 and 2 are not easy to obtain, and the operation is complicated, the reaction conditions are harsh, the cost is high, and there are potential safety hazards. At the same time, the environmental pollution is also large, and it is not suitable for industrial production.

Although the raw materials of synthetic route 3 are simple and easy to obtain, easy to operate, and suitable for industrial production, they need to be concentrated to obtain α-ketophenylalanine. High temperature in the later stage of concentration will easily lead to the decomposition of α-ketophenylalanine, and finally make the product yellow , there are many impurities, and multiple recrystallizations are required to obtain qualified products. At the same time, route 3 is a two-step reaction, which has low equipment utilization, takes up a lot of equipment, takes a lot of time, and the yield is low

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