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Recrystallization purification method of milrinone

A purification method and recrystallization technology, which is applied in the field of recrystallization purification of milrinone, can solve the problems of multiple DMF, poor crystallinity, and small crystal particles of the product, and achieve obvious technical effects, good crystallinity, and white color.

Inactive Publication Date: 2015-07-01
美信佳中维药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: the product is a light yellow crystal, and the color does not meet the medicinal requirements; DMF is relatively expensive and the cost is high; there may be more DMF in the purified product, which cannot meet the medicinal requirements
The problems of this method are: the amount of solvent used is too large, which brings a lot of inconvenience to the operation; the crystal particles of the refined product are small and the crystallinity is poor
But it also has the problem that the above-mentioned amount of solvent is too large, and the crystallinity is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The recrystallization purification method of milrinone comprises the following steps: adding a mixed solvent of 20 times the mass of the crude product to the crude product of milrinone, slowly heating to 60° C., until the crude product is completely dissolved, adding activated carbon with 15% of the mass of the crude product for decolorization for 1 hour, Suction filtration while hot, filter out activated carbon; cool the filtrate obtained by suction filtration to room temperature under slow stirring, crystallize, suction filtration again, wash with ethanol and suction filtration again, and then dry at 60°C to obtain off-white crystal; add the above-mentioned mixed solvent 20 times the mass of the white crystal to this type of white crystal, slowly heat to 60°C, wait until the almost white crystal is completely dissolved, cool to room temperature under slow stirring, and crystallize to obtain a white crystal. The white crystals are purified milrinone, with a content as h...

Embodiment 2

[0019] The recrystallization purification method of milrinone comprises the following steps: adding a mixed solvent of 18 times the mass of the crude product to the crude product of milrinone, slowly heating to 70° C., until the crude product is completely dissolved, adding activated carbon with 12% of the mass of the crude product for decolorization for 1.5 hours, Suction filtration while hot, filter out activated carbon; cool the filtrate obtained by suction filtration to room temperature under slow stirring, crystallize, suction filtration again, wash with ethanol and suction filtration again, and then dry at 65°C to obtain off-white crystal; add the above-mentioned mixed solvent 18 times the mass of the white crystal to this type of white crystal, slowly heat to 70 ° C, wait until the white crystal is completely dissolved, cool to room temperature under slow stirring, and crystallize to obtain a white crystal. The white crystals are purified milrinone, with a content as hig...

Embodiment 3

[0022] The recrystallization purification method of milrinone comprises the following steps: adding a mixed solvent of 15 times the mass of the crude product to the crude product of milrinone, slowly heating to 80° C., until the crude product is completely dissolved, adding activated carbon with 10% of the mass of the crude product for decolorization for 2 hours, Suction filtration while hot, filter out activated carbon; cool the filtrate obtained by suction filtration to room temperature under slow stirring, crystallize, suction filtration again, wash with ethanol and suction filtration again, and then dry at 70°C to obtain off-white crystals; add the above-mentioned mixed solvent 15 times the mass of the white crystals to this type of white crystals, slowly heat to 80 ° C, wait until the off-white crystals are completely dissolved, cool to room temperature under slow stirring, and crystallize to obtain white crystals. The above-mentioned white crystal is purified milrinone, t...

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Abstract

The invention relates to a recrystallization purification method of milrinone, belonging to the field of active pharmaceutical ingredient refinement. The method comprises the following steps: adding a mixed solvent into a milrinone crude product, slowly heating, dissolving, adding activated carbon for decolorization, and carrying out vacuum filtration while the solution is hot to remove the activated carbon; cooling the filtrate to room temperature while slowly stirring, crystallizing, carrying out vacuum filtration, washing the filter cake with ethanol, and drying to obtain a white-like crystal; and adding the mixed solvent into the white-like crystal, slowly heating until all the white-like crystal is dissolved, cooling to room temperature while slowly stirring, and crystallizing to obtain a white crystal which is the purified milrinone with the content of up to 99.90%. The mixed solvent composed of water, ethanol and DMF (N,N-dimethylformamide) is utilized for filtration and purification, thereby comprehensively satisfying the requirements for solvent consumption, crystallinity and content. The product provided by the invention has obviously better appearance (such as crystallinity and color) than the product in the prior art.

Description

technical field [0001] The invention relates to a purification method, in particular to a recrystallization purification method of milrinone. The invention belongs to the technical field of crude drug refining. Background technique [0002] Milrinone is a phosphodiesterase Ⅲ (PDE Ⅲ) inhibitor, which is the same drug as amrinone. Its mechanism of action is the same as that of amrinone. It is a drug for the treatment of heart failure. It is clinically used to treat patients with severe congestive heart failure and digitalis drug poisoning, and it has both positive inotropic and vasodilation effects. Compared with amrinone, the effect of milrinone is 10-30 times stronger, and the tolerance of the body is also better. In clinical application, milrinone is used for intravenous injection, so there are very high requirements for the purity and impurity control of the drug, which is also a hot direction in the research of milrinone synthesis in recent years. [0003] In the exist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/85
CPCC07D213/85C07B2200/13
Inventor 傅斌
Owner 美信佳中维药业股份有限公司
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