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Synthetic method of nisoldipine photolytic product reference substance

A synthetic method and technology of reference substances, applied in the direction of organic chemistry, etc., can solve the problems of long synthetic route, many reagents used, labor and environmental damage, etc., and achieve the effect of less environmental pollution, less toxic effect, and simple operation

Inactive Publication Date: 2009-01-21
药大制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] This route has the following disadvantages: (1) the synthesis route is long, (2) toxic reagents are used, which causes great harm to laborers and the environment, (3) more reagents are used

Method used

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  • Synthetic method of nisoldipine photolytic product reference substance

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Effect test

example 1

[0024] Nisoldipine 40g was made into a saturated solution of absolute ethanol. At room temperature, in an airtight container, the color changes from yellow to dark blue-green after three days of sunlight exposure. The solution was refluxed in a water bath for 30 minutes at a temperature of 70 degrees Celsius; the insoluble matter was filtered off while it was hot, and the filtrate was dried under reduced pressure at 50 degrees Celsius with a rotary evaporator. The resulting residue was recrystallized three times with absolute ethanol to obtain a refined product as a light blue-green powder.

example 2

[0026] Nisoldipine 80g was made into a saturated solution of absolute ethanol. At room temperature, in a closed container, after being irradiated by infrared light for 2 days, the color turns from yellow to dark blue-green. The solution was refluxed in a water bath for 20 minutes at a temperature of 75 degrees Celsius; while it was hot, the insoluble matter was filtered off with suction, and the filtrate was dried under reduced pressure at 60 degrees Celsius with a rotary evaporator. The resulting residue was recrystallized three times with absolute ethanol to obtain a refined product as a light blue-green powder.

example 3

[0028] Nisoldipine 70g was made into a saturated solution of absolute ethanol. At room temperature, in an airtight container, the color changes from yellow to dark blue-green after four days of exposure to sunlight. The solution was refluxed in a water bath for 50 minutes at a temperature of 80 degrees Celsius; the insoluble matter was filtered off while it was hot, and the filtrate was dried under reduced pressure at 70 degrees Celsius with a rotary evaporator. The resulting residue was recrystallized twice with ... to obtain the refined product as light blue-green powder.

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Abstract

A synthesis method of a control for the photolytic product of nisoldipine relates to the field of drug production. The method comprises the following steps that: 1) an absolute ethanol saturated solution of nisoldipine is irradiated with light in a closed container at room temperature, until the color turns from yellow to aquamarine blue and then keeps stable; 2) the obtained solution is refluxed in water bath for 20 to 40 minutes at 70 to 80DEG C, followed by the elimination of insoluble substances under the heat; 3) the obtained is dried at 50 to 70 DEG C and; 4) the obtained remnant are re-crystallized for 2 or 3 times to obtain the refined product, which appears to be a powder in pale aquamarine blue. The invention has the advantages of easy operation, no requirement of toxic reagents, minor toxic effects on human body, and minor pollution on environment.

Description

technical field [0001] The invention relates to the field of pharmacy, in particular to a method for synthesizing a nisoldipine photolysis product reference substance. Background technique [0002] Nisoldipine (I) is a dihydropyridine calcium antagonist, which can prevent the intake of calcium ions by cardiac muscle and vascular smooth muscle, has the effect of selectively expanding coronary arteries and peripheral blood vessels, improves myocardial blood supply, and reduces peripheral resistance, thereby Reduce myocardial oxygen consumption, enhance myocardial tolerance to hypoxia, and lower blood pressure in hypertensive patients. The drug has curative effect on coronary heart disease, hypertension and chronic congestive heart failure. Clinical studies have shown that the drug has no significant effect on the respiratory and central nervous system while causing a drop in blood pressure. Long-term treatment does not produce tolerance. The drug was pioneered by the German...

Claims

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Application Information

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IPC IPC(8): C07D211/90
Inventor 王卉孙颖
Owner 药大制药有限公司
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