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Stable protein kinase activator, and preparation method and purpose thereof

A protein kinase and activator technology, applied in the field of medicine, can solve the problem of no protein kinase activator - cyclic adenosine monophosphate preparation method and use, etc., and achieve the effect of good storage stability

Active Publication Date: 2011-11-23
刘力
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But so far, there is no novel and stable protein kinase activator reported in the literature at home and abroad—the hydrate of cyclic adenosine monophosphate and its preparation method and use

Method used

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  • Stable protein kinase activator, and preparation method and purpose thereof
  • Stable protein kinase activator, and preparation method and purpose thereof
  • Stable protein kinase activator, and preparation method and purpose thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Example 1 Preparation of magnesium salt 8 hydrate of cyclic adenosine monophosphate

[0078] In a 250ml three-necked flask, add 0.1mol of cyclic adenosine monophosphate, 100ml of water, stir, add 0.05mol of magnesium oxide, stir at 20-60°C for about 50 minutes to dissolve, filter, add 5 times the amount of acetone to make the solid Precipitation, cooling to about -10°C, standing for 24 hours, filtering, drying the solid at about 50°C for 4 hours to obtain 23.6g of off-white solid, melting point: 227°C decomposition (uncorrected), HPLC: cyclic adenosine monophosphate content 39.86%, Moisture is 17.57% as measured by Karl Fischer method, and thermal analysis: the weight loss of the platform is about 17.16% (see attached figure 1 ), which is within the error range with the result of the sample containing 8 crystal waters (theoretical value 17.48%); infrared spectrum: ν KBr max cm -1 3437, 3210, 2913, 2428, 1659, 1606, 1581, 1488, 1425, 1384, 1343, 1290, 1237, 1136, 1...

Embodiment 2

[0079] Example 2 Preparation of Cyclic Adenosine Monophosphate Calcium Salt 3.5 Hydrate

[0080] In a 250ml three-necked flask, add 0.1mol of purified cyclic adenosine monophosphate, 100ml of water, stir, add 0.05mol of calcium hydroxide or calcium oxide, stir at 20-60°C for about 60 minutes to dissolve, filter, Add 5 times the amount of absolute ethanol and isopropanol (1:1), cool to -10 ~ 5 ° C, stand for 24 hours, wait for the solid to precipitate, filter, and dry at about 50 ° C for 4 to 6 hours to obtain an off-white solid 19.2 grams, melting point: decomposition at 223°C (ELECTROTHERMAL MELTING POINT APPARATUS, uncorrected), infrared spectrum: Karl Fischer’s method determines that the water content is 8.52%, thermal analysis: the weight loss on the platform is about 8.4%, which is consistent with the result that the sample contains 3.5 crystal waters ( Theoretical value 8.30%) within the error range; ESI: m / z: 328; IR spectrum: ν KBr max cm -1 3436, 3209, 2913, 2428...

Embodiment 3

[0081] Example 3 Preparation of adenosine cyclophosphate meglumine monohydrate

[0082] Put 10g of purified cyclic adenosine monophosphate and equimolar meglumine into the reaction bottle, add 200ml of water, stir, control the temperature between 10-60°C, react for 10-120min, add 1% of the total solution Stir the activated carbon for half an hour and filter it, then filter it with a 0.22 micron microporous membrane, freeze it to -60~-40°C, keep it for about 4 hours, then raise the temperature to about -16°C, vacuum between 5-12Pa, vacuum Dry for about 20 hours, then vacuum-dry for about 4 hours at 20-30°C and vacuum degree 5-12Pa to obtain a white solid, which is easily soluble in water and has a melting point of 67-71.°C (ELECTROTHERMAL MELTING POINT APPARATUS , uncorrected); HPLC: cyclic adenosine monophosphate content is 60.79%, ESI: m / z: 523,328, 19,6, 195; moisture (Karl Fischer method): 3.51%, thermal analysis: platform weight loss is about 3.31%, which The result with ...

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Abstract

The invention relates to a novel stable protein kinase activator adenosine cyclophosphate derivative, which has good storage stability and preparation performance and can be applied to preparations of medicaments for treating or preventing human and mammal diseases, such as angina pectoris, heart failure, myocardial infarction, myocarditis, arrhythmia, acute leukemia, neurological diseases, respiratory system disease, senile chronic bronchitis, hepatitis and psoriasis, etc, and medicaments for improving symptoms of palpitaition, dyspnea and chest distress of rheumatic heart disease.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a stable protein kinase activator-cyclic adenosine monophosphate hydrate and its preparation and application. Background technique [0002] Cyclic adenosine monophosphate is a protein kinase activator and a derivative of nucleotides. It 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 regulate physiological functions and substance metabolism in cells, can change the function of cell membranes, and promote calcium ions in the sarcoplasmic substance to enter muscle fibers, thereby enhancing myocardial contraction and promoting the production of respiratory chain oxidases activity, improve myocardial hypoxia, relieve symptoms of coronary heart disease and im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/213C07H1/00A61K31/7076A61P9/10A61P9/04A61P9/00A61P9/06A61P19/02A61P35/02A61P25/00A61P11/00A61P1/16A61P17/06
CPCA61K31/7076C07H19/213A61P1/16A61P9/00A61P9/04A61P9/06A61P9/10A61P11/00A61P17/06A61P19/02A61P25/00A61P35/02
Inventor 刘力
Owner 刘力
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