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A kind of preparation method of nicorandil trimer

A technology of Nicorandil trimer and Nicorandil, which is applied in the field of preparation of Nicorandil trimer, can solve the difficulty of obtaining and limiting the research work of Nicorandil trimer impurities, Nicorandil Solve the problems of low yield of dil trimer and achieve the effect of good purity, fast acquisition and high yield

Active Publication Date: 2022-02-18
BURNING POINT (NANJING) BIOPHARMACEUTICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the acquisition of nicorandil trimer is mainly prepared from the nicorandil reaction solution by preparing the liquid phase. The yield of the prepared nicorandil trimer is low and the acquisition is difficult, which greatly limits the production capacity of nicorandil. The impurity research work of nicorandil trimer, therefore urgently need to find a kind of yield high, the preparation method of nicorandil trimer that is easy to separate

Method used

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  • A kind of preparation method of nicorandil trimer
  • A kind of preparation method of nicorandil trimer

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Decomposing Nikil (1.0 g) in DMA (2 mL), stirred at 100 ° C for 4.0 h at 100 ° C, slowly cooled to room temperature, slowly added carbon tetrachloride, stirring alfing, and a large amount of solid precipitation, filtration, Tetrahydrofuran washed with a crude product, and tetrahydrofuran was recrystallized to give a white solid Niul dimer nitrate 826.2 mg, purity 99.89%.

Embodiment 2

[0023] Dissolved Niki (1.0g) in DMA (3 mL), stirred at 90 ° C for 5.0 h at 90 ° C, slowly cooled to room temperature, slowly dropped chloroform, stirred, stirred with a large amount of solid, filtered, acetonitrile washing The crude product, acetonitrile was recrystallized to give a white solid Niul Trimer nitrate 837.4 mg, purity 99.91%.

Embodiment 3

[0025] Dissolis Nikil (1.0g) was dissolved in DMF (3 mL), stirred at 80 ° C for 6.0 h at 80 ° C, slowly cooled to room temperature, slowly added dichloromethane, stirred alfing, and a large amount of solid precipitation, Filtration The nitrile washed with a crude product, and the propionic nitrile was recrystallized to give a white solid Niul Trimer nitrate 855.9 mg, purity 99.93%.

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Abstract

The invention provides a preparation method of a nicorandil trimer, which comprises the following steps: (1) dissolving nicorandil in an organic solvent, stirring and reacting for 4‑7 h; Add the crystallization solvent dropwise to the liquid, slowly cool to room temperature, stir and crystallize, filter to obtain the crude product, and wash with organic solvent; (3) Add the above crude product into the recrystallization solvent, and after recrystallization, solid Nicorandil is obtained Trimeric nitrate. The preparation method of the nicorandil trimer disclosed by the invention can conveniently and quickly obtain the nicorandil trimer, and the obtained nicorandil trimer has a high yield and good purity.

Description

Technical field [0001] The present invention relates to the field of pharmaceutical chemistry, and more particularly to a method of preparing a Nikir trimer. Background technique [0002] Nicoran (Nicoandil) was developed by Japan Sino-foreign pharmaceutical company in 1984. Nikili is an anttrogologous drug, a nitrate compound, has permeability, increasing the intracellular calcium ion, increasing the permeability of the cell membrane on potassium ions, increasing coronary blood flow, inhibiting coronary artery spasm Role, when expanding the coronary blood vessel, does not affect blood pressure, heart rate, myocardial shrinkage, and myocardial oxygen consumption. Nikil also has the effect of inhibiting platelet aggregation to prevent thrombosis. Nikil, chemical name: N- (2-hydroxyethyl) nitrate, structural formula: [0003] [0004] The amount of active ingredient of the drug is an important symbol of the purity of drug purity, and the impurities in the drug directly affect the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/82
CPCC07D213/82
Inventor 林峰赵维唐亚军吴敏于学珍秦勇胡传良
Owner BURNING POINT (NANJING) BIOPHARMACEUTICAL TECH CO LTD
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