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Torasemide compound and new preparation method thereof

A technology of torsemide and compound, applied in the field of medicine, can solve the problems of low purity of torsemide and the like

Inactive Publication Date: 2011-06-01
HAINAN MEIDA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to overcome the defects of the above-mentioned prior art, especially the defect of low purity of torasemide prepared by the prior art, the present invention provides a new method for preparing torasemide, which is refined by torsemide, Obtain high-purity torasemide with high yield, improve the product quality of preparations, reduce toxic and side effects, ensure the quality of raw materials, and increase production yield

Method used

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  • Torasemide compound and new preparation method thereof
  • Torasemide compound and new preparation method thereof

Examples

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Effect test

Embodiment 1

[0057] The refining of embodiment 1 torasemide

[0058] Disperse 100g of crude torasemide in 1000ml of water to form an aqueous dispersion, then add dropwise 0.5mol / L sodium hydroxide solution to the aqueous dispersion until the pH value is 11, heat and stir at 95°C until clear, then add 1mol / L 200ml of ethanol solution of L sodium ethoxide was treated with stirring for 2 hours.

[0059] Then adjust the pH value to 6.0 with 1mol / L hydrochloric acid solution, precipitate solid, and filter.

[0060] Dissolve the precipitate in 800ml of water, add it to a fixed bed filled with D201 macroporous strongly basic styrene-based anion exchange resin, continue the exchange for 2.5 hours, then elute with 1.0mol / L sodium hydroxide solution, collect the eluate, Concentrate under reduced pressure.

[0061] Adjust the pH value to 6.0 with 0.5 mol / L acetic acid solution, precipitate solids, filter, wash with water 3 times, and dry under reduced pressure at 50°C for 6 hours to obtain 93.2 g...

Embodiment 2

[0062] The refining of embodiment 2 torasemide

[0063] Disperse 100g of crude torsemide in 1000ml of water to form an aqueous dispersion, then add dropwise 0.2mol / L sodium hydroxide solution to the aqueous dispersion until the pH value is 13, heat and stir at 89°C until clear, then add 1mol / L 200ml of ethanol solution of L sodium ethoxide was treated with stirring for 2 hours.

[0064] Then adjust the pH value to 6.0 with 1mol / L hydrochloric acid solution, precipitate solid, and filter.

[0065] Dissolve the precipitate in 800ml of water, add it to a fixed bed filled with D201 macroporous strongly basic styrene-based anion exchange resin, continue the exchange for 2.5 hours, then elute with 1.0mol / L sodium hydroxide solution, collect the eluate, Concentrate under reduced pressure.

[0066] Adjust the pH value to 6.0 with 0.5 mol / L phosphoric acid solution, precipitate solids, filter, wash with water 3 times, and dry under reduced pressure at 45°C for 10 hours to obtain 92...

Embodiment 3

[0067] The refining of embodiment 3 torasemide

[0068] Disperse 100g of crude torasemide in 2000ml of water to form an aqueous dispersion, then add dropwise 1mol / L sodium hydroxide solution to the aqueous dispersion until the pH value is 12, heat and stir at 90°C until clear, then add 1mol / L 200ml of ethanol solution of sodium ethoxide was stirred for 2 hours.

[0069] Then adjust the pH value to 6.0 with 0.5 mol / L hydrochloric acid solution, precipitate solid, and filter.

[0070] Dissolve the precipitate in 800ml of water, add it to a fixed bed filled with D201 macroporous strongly basic styrene-based anion exchange resin, continue the exchange for 2.5 hours, then elute with 1.0mol / L sodium hydroxide solution, collect the eluate, Concentrate under reduced pressure.

[0071] Use 0.5mol / L hydrochloric acid solution to adjust the pH value to 6.0, precipitate solid, filter, wash with water 3 times, and dry under reduced pressure at 50°C for 8 hours to obtain 93.4g of high-p...

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Abstract

The invention provides a torasemide compound and a new preparation method thereof, and the method comprises the following steps: (1) processing the torasemide raw material by alkali metals or alkaline earth metal alkane oxides with the presence of an appropriate solvent or solvent mixture under an alkaline and heating condition; (2) adjusting the pH value by an appropriate acid; (3) adsorbing the torasemide by strong basic ion exchange resin and eluting the product; (4) adjusting the pH value by an appropriate acid to obtain a three-stage purified torasemide. The preparation method of torasemide improves the product quality of the preparation, reduces the toxic and side effects, is simple and easy to operate, and is applicable to large-scale industrial production.

Description

technical field [0001] The invention relates to a torasemide compound and a new preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Torasemide (English name: Torasemide), its chemical name is: N-[[(1-methylethyl)amino]carbonyl]-4-[(3-methylphenyl)amino]-3-pyridine Sulfonamide, molecular formula: C 16 h 20 N 4 o 3 S, molecular weight: 348.43, structural formula: [0003] [0004] Torsemide is a new generation of high-efficiency loop diuretics. It was launched in Germany in 1993 and in the United States in the following year. In 2004, my country's SFDA approved the production of the first domestic torsemide aqueous injection preparation (Tesuni). Torsemide is a sulfonylurea pyridine diuretic that acts on the thick ascending limb of Henle's loop of Henle and inhibits Na + / K + / 2Cl - Carrier system that makes urine Na + , Cl - and water excretion increased, but had no significant effect on glomerular filtration ra...

Claims

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Application Information

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IPC IPC(8): C07D213/74
Inventor 廖爱国
Owner HAINAN MEIDA PHARMA
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