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A kind of preparation method of Regardson crystal form e

A technology of regadeson and crystal form, which is applied in the field of preparation of regadeson crystal form E, and can solve the problem of low purity of crystal form E

Active Publication Date: 2018-10-02
SHANGHAI ZIYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the purity of the crystal form E obtained by this preparation method is not high

Method used

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  • A kind of preparation method of Regardson crystal form e
  • A kind of preparation method of Regardson crystal form e
  • A kind of preparation method of Regardson crystal form e

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Experimental program
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preparation example Construction

[0036] The invention discloses a method for preparing crystal form E of regadepine, and those skilled in the art can learn from the content of this article and appropriately improve the process parameters to realize it. In particular, it should be pointed out that all similar replacements and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The method and application of the present invention have been described through preferred embodiments, and the relevant personnel can obviously make changes or appropriate changes and combinations to the method and application described herein without departing from the content, spirit and scope of the present invention to realize and Apply the technology of the present invention.

[0037] The abbreviations and English specific meanings used in the specification and claims are as follows:

[0038] Abbreviation and English meaning

[0039] DMSO N,N-Dimethylsulfoxide...

Embodiment 1

[0052] Embodiment 1 Preparation of Regardson Crystal Form E

[0053] Dissolve 40 mg of regadenoson in 2 mL of DMSO to obtain a 20 mg / mL solution. Filter through a 0.45μm filter membrane, and inject the liquid into the 2mL quantitative loop of the reversed-phase chromatography system through the injection needle. The reversed-phase chromatography conditions are: chromatographic column is C18, 250×4.6mm; UV wavelength is 254nm; It is acetonitrile, phase A is water phase, and the flow rate is 1mL / min; the gradient elution method is adopted, and the gradient elution procedure is as follows:

[0054] time

B phase ratio

0-5min

5％

5-10min

5％-10％

10-20min

15％

20-40min

15％-50％

40-45min

50％-90％

[0055] Separation was carried out according to the above established procedure, and the main peak sample with a retention time of 30 min was collected to obtain a mixture of acetonitrile and water. Add 10 mL of dichloromethan...

Embodiment 2

[0064] Embodiment 2 Preparation of Regardson crystalline form E

[0065] Dissolve 10 mg of regadenoson in 1 mL of DMF to obtain a 27 mg / mL solution. Filter through a 0.45μm filter membrane, and inject the liquid into the 2mL quantitative loop of the reversed-phase chromatography system through the injection needle. The reversed-phase chromatography conditions are: chromatographic column is C18, 250×4.6mm; UV wavelength is 254nm; It is acetonitrile, phase A is water phase, and the flow rate is 1mL / min; the gradient elution method is adopted, and the gradient elution procedure is as follows:

[0066] time

[0067] Separation was carried out according to the above established procedure, and the main peak sample with a retention time of 30 min was collected to obtain a mixture of acetonitrile and water. Add 50 mL of ethyl acetate to the obtained mixture, separate the organic phase, concentrate under reduced pressure at 30°C, add 1 mL of DMF to the residue, dissolve it, ...

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Abstract

The invention relates to the field of crystal form preparation, in particular to a preparing method for a regadenoson crystal form E. The preparing method includes the steps that regadenoson and first organic solvent are mixed and purified through reversed-phase high-performance liquid chromatography, and the component with the retention time of 30 min is collected to obtain a first intermediate product; the first intermediate product is mixed with second organic solvent to obtain an organic phase, and a second intermediate product is obtained through concentration; the second intermediate product and DMF are mixed and crystallized to obtain the regadenoson crystal form E. The purity of the regadenoson crystal form E can be improved greatly by means of the preparing method.

Description

technical field [0001] The invention relates to the field of preparation of crystal forms, in particular to a method for preparing crystal form E of regadepine. Background technique [0002] Myocardial perfusion imaging (MPI) is a useful diagnostic technique for the detection and characterization of coronary artery disease. Perfusion imaging uses substances such as radionuclides to identify areas of insufficient blood flow. In MPI, blood flow at rest is measured and compared to blood flow measured during treadmill exercise (cardiac stress test). Many patients are unable to provide adequate blood flow for cardiac stress testing due to factors such as peripheral vascular disease. Therefore, agents that increase cardiac blood flow for a short period of time are essential, especially agents that do not cause peripheral vasodilation. [0003] Adenosine is a potent vasodilator by interacting with adenosine receptors (characterized as subtype A 1 、A 2A 、A 2B and A 3 adenosin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H19/167C07H1/06
Inventor 刘伟张志刚任真
Owner SHANGHAI ZIYUAN PHARMA
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