Milrinone salt preparation method and its uses

A technology of milrinone and hydrochloric acid, applied in the fields of chemical industry and chemical medicine, can solve the problems of inconvenient transportation, difficult storage, poor stability, etc., and achieve the effect of solving the problems of solubility and stability, and being convenient for storage and transportation.

Inactive Publication Date: 2007-04-25
INST OF PHARMACY SHANDONG PROV ACAD OF MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since milrinone lactate is an aqueous injection, the disadvantages in the actual application process are: poor stability, difficult to store, and inconvenient to transport

Method used

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  • Milrinone salt preparation method and its uses
  • Milrinone salt preparation method and its uses
  • Milrinone salt preparation method and its uses

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: the preparation of milrinone sodium salt

[0032] Put 10g of milrinone in a 500ml beaker, add dropwise 0.1N sodium hydroxide aqueous solution and stir to dissolve it until the pH value is 7-8, add acetone 5 times the volume of the solution, cool, and precipitate a white precipitate, filter, filter The cake was washed twice with acetone, dried in air, and then dried at 105° C. for 2 hours to obtain 10.16 g of milrinone sodium salt with a yield of 92%.

[0033] Elemental Analysis: C 12 h 8 N 3 ONa, calculated C: 61.74% H: 3.43% N: 18.01% Na: 9.86%, experimental value C: 61.70% H: 3.38% N: 17.94% Na: 9.83%;

[0034] Infrared spectrum (KBr, cm -1 ): 3636 3264 3057 2214 1594 1550 1522 14821400 1367 1259 827 807 789 601

[0035] UV absorption spectrum: determination of maximum lambda in aqueous solution max 333nm, 269nm.

Embodiment 2

[0036] Embodiment 2. Preparation of milrinone potassium salt

[0037] Put 10g of milrinone in a 500ml beaker, add 0.1N potassium hydroxide solution dropwise and stir to dissolve it until the pH value of the solution is 7-8, add acetone 5 times the volume of the solution, cool, and precipitate a white precipitate, filter, The filter cake was washed twice with acetone, dried in air, and then dried at 105° C. for 2 hours to obtain 5.0 g of milrinone potassium salt, and 4.5 g was recovered from the mother liquor, with a yield of 80.5%.

[0038] Elemental Analysis: C 12 h 8 N 3 OK, calculated value C: 57.78% H: 3.21% N: 16.85% K: 15.64%, experimental value C: 57.63% H: 3.23% N: 16.80% K: 15.60%

[0039] Infrared spectrum (KBr, cm -1 ): 3335 3032 2213 1596 1549 1525 1480 13981367 1270 1226 830 790 597

[0040] UV absorption spectrum: determination of maximum lambda in aqueous solution max 334nm, 266nm.

Embodiment 3

[0041] Embodiment 3. The preparation of milrinone hydrochloride

[0042] Put 10g of milrinone in a 500ml beaker, add dropwise 0.1N hydrochloric acid solution and stir to dissolve it, so that the pH of the solution is 4-4.5, add acetone 5 times the volume of the solution, cool, and precipitate a white precipitate, filter, filter cake Wash twice with acetone, dry in air, and then dry at 105° C. for 2 hours to obtain 12 g of milrinone hydrochloride with a yield of 93%.

[0043] Elemental analysis; C 12 h 9 N 3 O HCl, calculated value C: 58.11% H: 4.07% N: 16.56% Cl: 14.31%, experimental value C: 58.11% H: 4.07% N: 16.56% Cl: 13.98%

[0044] Infrared spectrum (KBr, cm -1 ): 3223 3026 2987 2784 2627 2235 1873 1654 1626 1570 1511 1478 1371 1336 1182 1031 830 687 583

[0045] UV absorption spectrum: determination of maximum lambda in aqueous solution max 331nm, 265nm.

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Abstract

The invention discloses a preparing method of Milinong salt and application in the lyophilized product, which is characterized by the following: adopting refined Milinong as raw material; reacting with alcaine, phosphoric acid, sulfuric acid, methanesulfonic acid, sodium hydroxide and potassium hydroxide to obtain the soluble product; blending soluble Milinong salt and auxiliary material to form injection lyophilized product.

Description

1. Technical field [0001] The invention relates to a preparation method of a medicine and an application thereof, in particular to a preparation method of a salt of milrinone and an application thereof, and belongs to the fields of chemical industry and chemical medicine. 2. Background technology [0002] Milrinone, English name Milrinone, chemical name 2-methyl-6-oxo-1,6-dihydro-[3,4'bipyridine]-5-carbonitrile, is a white solid, it was listed in the United States in 1987 The second-generation bispyridine cardiotonic drug, the drug selectively inhibits phosphodiesterase III in myocardial cells, increases intracellular cyclic adenosine monophosphate (C-AMP), and changes the movement of intracellular and extracellular calcium, thereby increasing myocardial Contractility, its cardiotonic activity is 20 times that of the homologue amrinone, and the adverse reactions are small. However, because milrinone itself is insoluble in water, the current clinical milrinone injection prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/85A61K31/444A61K9/19A61P9/04
Inventor 薛克亮刘爱芹
Owner INST OF PHARMACY SHANDONG PROV ACAD OF MEDICAL SCI
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