A kind of preparation method of nisoldipine impurity

A nisoldipine and impurity technology, which is applied in the field of preparation of nisoldipine impurities, can solve the problems of no drug efficacy and toxicity of the product, poor stability of nisoldipine, etc., and achieve the effects of high yield, low production cost, and simple processing method

Active Publication Date: 2022-03-08
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, nisoldipine has poor stability and is easy to decompose when exposed to light, and the decomposed products have no drug effect and are highly toxic

Method used

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  • A kind of preparation method of nisoldipine impurity
  • A kind of preparation method of nisoldipine impurity
  • A kind of preparation method of nisoldipine impurity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Take 1g of nisoldipine, add 10mL of ethanol to dissolve;

[0032] (2) Add 15 mg of free radical initiator 2,2-2,2-azobisisobutyronitrile (AIBN) to the solution to obtain a reaction solution;

[0033] (3) Place the reaction solution under a fluorescent lamp with a power of 30w, irradiate and stir for 35h;

[0034] (4) Add 100 mL of water to the solution obtained in step (3), filter out the solid, and separate the product from the filtrate by column chromatography.

[0035] The solid sample of the product obtained in Example 1 above was dissolved in ethanol and left to stand for 7 days, and a blue-green prismatic single crystal was precipitated. The single crystal is subjected to X-ray single crystal diffraction, and the obtained crystal structure is as follows figure 1 As shown, the crystal structure belongs to the triclinic crystal system, the space group is P-1, (4), α / °=90.963 (2) β / °=98.659 (2) γ / °=108.680 (2) V=941.26 (4) Z=2.

[0036] The product obtained ...

Embodiment 2

[0041] (1) Take 1g nisoldipine, add 20mL acetone to dissolve;

[0042] (2) 15 mg of free radical initiator 1,2,4,5-tetracyanobenzene (TCNB) was added to the solution to obtain a reaction solution;

[0043] (3) Place the reaction solution under a fluorescent lamp with a power of 30w, irradiate and stir for 15h;

[0044] (4) Add 100 mL of water to the solution obtained in step (3), filter out the solid, and separate the product from the filtrate by column chromatography.

Embodiment 3

[0046] (1) Take 1g of nisoldipine, add 5mL of ethanol and 10mL of acetone to dissolve;

[0047] (2) Add 10 mg of free radical initiator 2,2-2,2-azobisisobutyronitrile (AIBN) to the solution to obtain a reaction solution;

[0048] (3) Place the reaction solution under a fluorescent lamp with a power of 30w, irradiate and stir for 5h;

[0049] (4) Add 100 mL of water to the solution obtained in step (3), filter out the solid, and separate the product from the filtrate by column chromatography.

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Abstract

The invention discloses a preparation method of nisoldipine impurity. The nisoldipine impurity is 2,6-dimethyl-4-(2-nitrosophenyl)-1,4-dihydro-3,5-pyridinedicarboxylate methyl isobutyl ester, the structure is as follows: Ⅰ) as shown. The preparation method of the nisoldipine impurity is prepared by taking nisoldipine as a raw material, adding a free radical initiator, and undergoing one-step photodegradation. The method adopted in the present invention is simple, easy to operate, mild in reaction conditions, and simple in post-treatment process, and provides a new way for further identifying, separating, preparing and characterizing the nisoldipine impurities, improving the quality control level and medication safety of nisoldipine, It is beneficial to the control of the quality of medicines in the production process.

Description

technical field [0001] The invention relates to a preparation method of nisoldipine impurities, belonging to the technical field of drug synthesis. Background technique [0002] Nisoldipine, yellow crystalline powder, chemical name: 2,6-dimethyl-4-(2-nitrophenyl)-1,4-dihydro-3,5-pyridinedicarboxylic acid methyl ester iso Butyl ester, molecular formula C 20 h 24 N 2 o 6 , molecular weight 388.41. [0003] Nisoldipine is currently the long-acting dihydropyridine calcium antagonist with the strongest selective vasodilation effect. It has significant medicinal effect on preventing coronary heart disease, hypertension and chronic congestive heart failure, and can reduce the risk of fatal ventricular fibrillation caused by acute myocardial infarction. Pharmacokinetic studies of different animals have shown that it is absorbed quickly and completely in the body, and has the longest duration. The plasma elimination half-life is as long as 42 to 54 hours. Effective drug in typ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/90
CPCC07D211/90C07B2200/13
Inventor 王明亮王萌从扬杜存彬江周宇邢可李晓萱卞宇超
Owner SOUTHEAST UNIV
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