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Method for preparing alpha-calcium picrolonate

A technology of calcium keto acid and keto acid, applied in the field of preparation of calcium α-keto acid, can solve problems such as environmental pollution and increase cost, and achieve the effect of easy separation and purification

Inactive Publication Date: 2010-06-30
YANGTZE RIVER PHARMA GRP BEIJING HAIYAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the reaction of α-keto acid with calcium chloride will release toxic gas hydrogen chloride, which must be neutralized by adding alkali, causing environmental pollution and increasing the cost

Method used

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  • Method for preparing alpha-calcium picrolonate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0019] At 25°C, 69.6 grams, 0.6 moles of 3-methyl-2-oxobutanoic acid were added to a 1000ml three-necked flask, 400ml of purified water was added, stirred, the pH value was adjusted to 5 with calcium carbonate, and the stirring was continued for one hour. After the reaction was completed, the reaction solution was extracted with 200 ml of ethyl acetate, and the organic layer was concentrated to recover unreacted acid. The aqueous layer was concentrated to dryness, and the residue was crystallized with water to obtain 57.2 g of a white solid, with a yield of 70.6%.

Embodiment 2

[0021] At 25°C, add 130 grams, 1 mole of 4-methyl-2-oxopentanoic acid into a 1000ml three-necked flask, add 700ml of purified water, stir, adjust the pH value to 4.5 with calcium bicarbonate, and continue stirring for one hour . After the reaction was completed, the reaction solution was extracted with 350 ml of ethyl acetate, and the organic layer was concentrated to recover unreacted acid. The aqueous layer was concentrated to dryness, and the residue was crystallized with water to obtain 121 g of a white solid with a yield of 81.2%.

Embodiment 3

[0023] At 25°C, add 130 grams, 1 mole of 3-methyl-2-oxopentanoic acid into a 1000ml three-necked flask, add 700ml of purified water, stir, adjust the pH value to 5 with calcium carbonate, and continue stirring for one hour. After the reaction was completed, the reaction solution was extracted with 350 ml of ethyl acetate, and the organic layer was concentrated to recover unreacted acid. The aqueous layer was concentrated to dryness, and the residue was crystallized with water to obtain 116 g of a white solid with a yield of 77.9%.

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Abstract

The invention relates to a method for preparing alpha-calcium picrolonate, which comprises the following steps of: adding alpha-ketonic acid into a proper amount of water; adjusting a PH value to 3-6 by using calcium carbonate or calcium bicarbonate; controlling the temperature to be 0-40 DEG C; concentrating, crystallizing and obtaining the product alpha-calcium picrolonate. The process is simple, is easy for operation, can finish reaction in one step and has high product yield and high quality without producing other by-products and can be used for the industrialized production of the alpha-calcium picrolonate.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to the preparation method of α-ketoacid calcium. Background technique [0002] α-keto acids are important products of animal and plant metabolism, and are also important intermediates for the synthesis of various useful organic compounds such as α-amino acids and α-hydroxy acids. The α-keto acid salt can be effectively used in the treatment of chronic renal failure-uremia and other diseases, which is of great significance to the development of drugs. Calcium α-ketoacids, compared to sodium α-ketoacids, are particularly important in terms of the large reduction in cations in the ion balance, which is particularly critical for kidney disease. [0003] Therefore, it is desirable to have a simple, high-yield, and economical method that can easily produce these calcium salts of α-ketoacids on a large scale. [0004] There are several methods in the prior art for the preparation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/185C07C51/41
Inventor 张培龙石和鹏侯鹏宋志涛李玉宽
Owner YANGTZE RIVER PHARMA GRP BEIJING HAIYAN PHARMA
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