Preparation method of Regadenoson of crystal form B

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

Active Publication Date: 2015-12-23
SHANGHAI ZIYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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

Method used

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  • Preparation method of Regadenoson of crystal form B
  • Preparation method of Regadenoson of crystal form B
  • Preparation method of Regadenoson of crystal form B

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preparation example Construction

[0035] The present invention discloses a preparation method of Ruijia Desson crystal form B, and those skilled in the art can learn from the content of this article and appropriately improve the process parameters to achieve. 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 deemed to be included in the present invention. The method and application of the present invention have been described through the preferred embodiments. It is obvious that relevant personnel can modify or appropriately change and combine the methods and applications described herein without departing from the content, spirit and scope of the present invention to achieve and Apply the technology of the present invention.

[0036] The abbreviations used in the specification and claims and the specific meanings in English are as follows:

[0037]

[0038]

[0039] The raw materials or reagents used in the preparation...

Embodiment 1

[0046] Example 1 Preparation of Rega Desson Form B

[0047] Dissolve 40 mg of Regadesone in 2 mL of DMSO to obtain a 20 mg / mL solution. Filtered with a 0.45μm filter membrane, the liquid is injected into the 2mL quantitative loop of the reversed-phase chromatography system through the injection needle. The reversed-phase chromatographic conditions are: the column is C18, 250×4.6mm; the ultraviolet wavelength is 254nm; the mobile phase, phase B It is acetonitrile, phase A is the water phase, and the flow rate is 1 mL / min; the gradient elution method is adopted, and the specific gradient elution procedure is:

[0048] Time

B phase

0-5min

5％

5-10min

5％-10％

10-20min

15％

20-40min

15％-50％

40-45min

50％-90％

[0049] Separate according to the above established procedure, collect the main peak sample with a retention time of 15 minutes, and obtain a mixture of acetonitrile and water. 10 mL of dichloromethane was added to the obtained mixed solution, and the organic phase was...

Embodiment 2

[0058] Example 2 Preparation of Rega Desson Form B

[0059] Dissolve 10 mg of Regadesone in 1 mL of DMF to obtain a 27 mg / mL solution. Filtered with a 0.45μm filter membrane, the liquid is injected into the 2mL quantitative loop of the reversed-phase chromatography system through the injection needle. The reversed-phase chromatographic conditions are: the column is C18, 250×4.6mm; the ultraviolet wavelength is 254nm; the mobile phase, phase B It is acetonitrile, phase A is the water phase, and the flow rate is 1 mL / min; the gradient elution method is adopted, and the specific gradient elution procedure is:

[0060] Time

[0061] Separate according to the above established procedure, collect the main peak sample with a retention time of 15 minutes, and obtain a mixture of acetonitrile and water. 50 mL of ethyl acetate was added to the obtained mixed solution, and the organic phase was separated and concentrated under reduced pressure at 30°C. 1 mL of trifluoroethanol was added t...

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Abstract

The invention relates to the field of crystal form preparation, and especially relates to a preparation method of Regadenoson of crystal form B. The preparation method comprises the following steps: taking Regadenoson, mixing Regadenoson with a first organic solvent, carrying out reversed-phase high performance liquid chromatography purification, and collecting a component with the retention time of 15min to obtain a first intermediate; mixing the first intermediate with a second organic solvent to obtain an organic phase, and concentrating to obtain a second intermediate; and mixing the second intermediate with trifluoroethyl alcohol, and crystallizing to obtain the Regadenoson of crystal form B. The preparation method can greatly improve the purity of the Regadenoson of crystal form B.

Description

Technical field [0001] The invention relates to the field of crystal form preparation, and in particular to a method for preparing Regadesson crystal form B. Background technique [0002] Myocardial perfusion imaging (MPI) is a useful diagnostic technique for the detection and characterization of coronary heart disease. Perfusion imaging uses substances such as radionuclides to identify areas of insufficient blood flow. In MPI, the blood flow at rest is detected and the result is compared with the blood flow detected during a treadmill exercise (heart stress test). Many patients are unable to provide sufficient blood flow for cardiac stress tests due to peripheral vascular diseases. Therefore, drugs that increase cardiac blood flow in a short period of time are indispensable, especially drugs that do not cause peripheral vasodilation. [0003] Adenosine is a potent vasodilator, it interacts with adenosine receptors (characterized as subtype A 1 , A 2A , A 2B And A 3 The family o...

Claims

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Application Information

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