A kind of crystallization method of 3′,5′-cyclic adenosine monophosphate

A technology of cyclic adenosine monophosphate and cyclic adenosine monophosphate, applied in the 3' field, can solve the problems of low yield and poor product quality, and achieve the effects of high crystallization yield, low cost and good repeatability

Active Publication Date: 2011-12-07
NANJING BIOTOGETHER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Therefore, the object of the present invention is to provide a new high-yield 3', the crystallization method of 5'-cyclic adenosine monophosphate, adopting the crystallization technology combining reaction-low temperature to replace solvent strong analysis method and freeze-drying method, To overcome the shortcomings of poor product quality and low yield in the existing 3', 5'-cyclic adenosine monophosphate crystallization technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Use 5M ammonia water to react with 3',5'-cyclic adenosine monophosphate aqueous solution to generate 0.95L of 3',5'-cyclic adenosine monophosphate ammonium salt solution with a concentration of 187g / L, control the pH to 8.0, and place it in a crystallization tank. Control the stirring speed at 150rpm at 30°C, and slowly add a phosphoric acid solution with a concentration of 2M at a flow rate of 0.2% / min (i.e. 1.9mL / min) of the volume of the initial 3',5'-cyclic adenosine monophosphate ammonium salt solution until When the pH value is 2.0, stop adding acid, lower the temperature to 5°C, and store for 20 hours. After the crystallization is complete, filter the suspension, wash the white crystals with ethanol, and dry them in vacuum to obtain 3',5'-cyclic adenosine mono Phosphoric acid crystals were 166.1 g, the crystallization yield was 93.5%, and the purity was 99.4%.

Embodiment 2

[0036] Use 3M ammonia water to react with 3', 5'-cyclic adenosine monophosphate aqueous solution to generate a concentration of 105g / L 3', 5'-cyclic adenosine monophosphate ammonium salt solution 1L, control pH 7.0, place in crystallization tank, Control the stirring speed at 200rpm at 35°C, and slowly add a sulfuric acid solution with a concentration of 3M at a flow rate of 0.4% / min (ie 4mL / min) of the volume of the initial 3',5'-cyclic adenosine monophosphate ammonium salt solution until the pH value When the temperature is 2.5, stop adding acid, lower the temperature to 5°C, and store for 18 hours. After the crystallization is complete, filter the suspension with suction, wash the white crystals with ethanol, and dry them in vacuum to obtain 3',5'-cyclic adenosine monophosphate crystals. 96.71g, the crystallization yield is 92.10%, and the purity is 99.4%.

Embodiment 3

[0038] Use 3M sodium hydroxide to react with 3',5'-cyclic adenosine monophosphate aqueous solution to generate 1.5L of 3',5'-cyclic adenosine monophosphate sodium salt solution with a concentration of 185g / L, control the pH to 8.0, and place it in a crystallization tank , at 30°C, the stirring speed was controlled at 200rpm, and the sulfuric acid solution with a concentration of 2M was slowly added at a flow rate of 0.4% / min (ie 6mL / min) of the volume of the initial 3',5'-cyclic adenosine monophosphate sodium salt solution, Stop adding acid until the pH value is 2.0, lower the temperature to 5°C, and store for 20 hours. After the crystallization is complete, filter the suspension with suction, wash the resulting white crystals with ethanol, and dry them in vacuum to obtain 3',5'-cyclic adenosine Monophosphoric acid crystals were 256.97g, the crystallization yield was 92.6%, and the purity was 99.3%.

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Abstract

Provided is a crystallization process of cyclic adenosine 3′,5′-monophosphate, which comprises the following steps: 1) reacting an aqueous solution of cyclic adenosine 3′,5′-monophosphate with a base to obtain a salt of cyclic adenosine 3′,5′-monophosphate; 2) reacting the cyclic adenosine 3′,5′-monophosphate salt solution obtained in step 1) with an acid to obtain cyclic adenosine 3′,5′-monophosphate; 3) keeping cyclic adenosine 3′,5′-monophosphate obtained in step 2) at 0-15° C.

Description

technical field [0001] The invention belongs to the technical field of crystallization, and in particular relates to a crystallization method of 3', 5'-cyclic adenosine monophosphate. Background technique [0002] 3', 5'-cyclic adenosine monophosphate (3', 5'-cyclic adenosine monophosphate) is a protein kinase activator and a derivative of nucleotides. 3',5'-cyclic adenosine monophosphate is an important substance with physiological activity that widely exists in the human body. It is produced by adenosine triphosphate under the catalysis of adenylyl cyclase and can regulate various functional activities of cells. As the second messenger of hormones, hormones can regulate physiological functions and substance metabolism in cells, can change the function of cell membranes, and promote calcium ions in the reticulum sarcoplasm to enter muscle fibers, thereby enhancing myocardial contraction and promoting oxygenation of the respiratory chain Enzyme activity can improve myocardi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/213C07H1/06
CPCC07H1/06C07H19/16C07H19/213
Inventor 应汉杰钱文斌陈勇陈晓春柏建新熊健林晓清
Owner NANJING BIOTOGETHER
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