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Method for crystallizing milrinone

A milrinone and crystallization technology, applied in the direction of organic chemistry, can solve problems such as unsatisfactory effects, achieve the effects of increased yield and purity, simple process, and solvent saving

Inactive Publication Date: 2012-07-11
方晏燕
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] It can be seen that the existing literature records all use recrystallization or different single solvent treatment, but the effect is not satisfactory

Method used

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  • Method for crystallizing milrinone
  • Method for crystallizing milrinone
  • Method for crystallizing milrinone

Examples

Experimental program
Comparison scheme
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Embodiment Construction

[0013] After the reaction in the last step of milrinone synthesis, add dimethylformamide (DMF) equivalent to 5 to 10 times the volume of milrinone to the crude product of milrinone, slowly heat to dissolve, and then re- Add hot water (60 to 100°C) equal to the volume of dimethylformamide (DMF), preferably 80-95°C, the addition of hot water significantly increases the dissolution rate and solubility of milrinone, and slowly stir to cool down to room temperature Crystals were precipitated, and suction filtration was performed, the filter cake was washed with a small amount of water, and the filter cake was vacuum-dried at 70-80°C to obtain white crystals.

[0014] The temperature of the hot water in the above dissolution process, after long-term practice and exploration by the applicant, is 90°C which is the most suitable. At this time, the dissolution rate increases significantly, which can quickly and fully dissolve milrinone in the solvent to obtain a transparent and clear sol...

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Abstract

The invention provides a method for crystallizing milrinone without recrystallizing. A mixed solvent is used, and hot water is added to dimethyl formamide (DFM), thus the defects of multiple re-crystallization low crystal purity due to the utilization of signal solvent in the prior art are overcome. In the last step of subjecting materials to reaction to synthesize the milrinone, the crystallization is carried out to obtain the milrinone with a good crystal form, higher purity and higher yield, thus the operation and the reaction process are simplified, the pollution is reduced, and the cost is lowered. The milrinone is suitable for large-scale industrial production as the active pharmaceutical ingredient and meets the requirement of the injection preparation.

Description

technical field [0001] The application relates to a crystallization method of milrinone, which belongs to the crystallization method of specific drugs. Background technique [0002] Milrinone (milrinone) is a drug for the treatment of heart failure, which can be used clinically for the treatment of heart failure patients with severe congestive heart failure or digitalis poisoning. Milrinone, as a non-digital and non-catecholamine cardiotonic drug, has both positive inotropic and vasodilation effects, because it can enhance myocardial contractility and increase cardiac output, while reducing cardiac load without Increase myocardial oxygen consumption, thereby improving cardiac function in patients with severe congestive heart failure or digitalis poisoning, and reducing dyspnea, cyanosis and pulmonary rales. In clinical applications, milrinone is generally used by intravenous injection, so as a drug that can be used as an emergency and administered intravenously, there are v...

Claims

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Application Information

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IPC IPC(8): C07D213/85
Inventor 方晏燕程宜兴贺学林刁何芳
Owner 方晏燕
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