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Preparation method of anhydrous dextro lansoprazole

A technology of dexlansoprazole and dexlansoprazole hydrate, applied in the field of preparation of anhydrous dexlansoprazole, can solve the problem of poor sample stability, poor water removal effect, dexlansoprazole The water content of azoles does not meet the requirements and other problems, and achieves the effect of simple operation, good stability and low energy consumption

Active Publication Date: 2017-12-12
南京博德生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

D-lansoprazole hydrate is suspended in methyl tert-butyl ether, heated and refluxed to separate water to separate out solids, and the color of dex-lansoprazole obtained by this method is brown, and the sample stability is poor; suspended in ether solvents, cooled and crystallized to obtain Anhydrous dexlansoprazole, if the crystal water contained in the dexlansoprazole hydrate or the free water content of the method is greater than 5%, the water content of the obtained dexlansoprazole does not meet the requirements. Ineffective

Method used

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  • Preparation method of anhydrous dextro lansoprazole
  • Preparation method of anhydrous dextro lansoprazole
  • Preparation method of anhydrous dextro lansoprazole

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Experimental program
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Effect test

Embodiment 1

[0029] Weigh D-lansoprazole hydrate (water content 7.5%, 8g) and suspend it in isopropyl ether (40mL), stir at room temperature evenly, concentrate under reduced pressure at 35°C to dryness, add isopropyl ether (40mL), stir evenly Concentrate under reduced pressure to dryness, add isopropyl ether (40mL) again, stir evenly, concentrate under reduced pressure to dryness, add isopropyl ether (40mL), stir and beat at room temperature for 30 minutes, suction filter, wash with isopropyl ether, collect and filter The cake was vacuum-dried at 25° C. for 8 hours to obtain 7.17 g of anhydrous D-lansoprazole as a white solid, with a yield of 89.6% and a water content of 0.49%.

Embodiment 2

[0031] Weigh D-lansoprazole hydrate (water content 7%, 8g) and suspend it in ether (40mL), stir evenly at room temperature, concentrate under reduced pressure at 25°C to dryness, add ether (40mL), stir evenly and concentrate under reduced pressure To dryness, diethyl ether (40 mL) was added again, stirred evenly, concentrated to dryness under reduced pressure, diethyl ether (40 mL) was added, stirred and beaten at room temperature for 30 minutes, suction filtered, washed with diethyl ether, the filter cake was collected, and vacuum-dried at 25°C for 8 hours. Obtained 7.27 g of anhydrous dexlansoprazole in the form of a white solid, with a yield of 90.9% and a water content of 1.70%.

Embodiment 3

[0033] Weigh D-lansoprazole hydrate (water content 15%, 10g) and suspend it in methyl tert-butyl ether (50mL), stir evenly at room temperature, concentrate to dryness under reduced pressure at 28°C, add methyl tert-butyl ether (50mL), stirred evenly, concentrated to dryness under reduced pressure, added methyl tert-butyl ether (50mL) again, stirred evenly, concentrated to dryness under reduced pressure, added methyl tert-butyl ether (50mL), stirred and beat at room temperature for 30 minutes , filtered with suction, washed with methyl tert-butyl ether, collected the filter cake, and vacuum-dried for 8 hours at 25°C to obtain 8.36g of anhydrous D-lansoprazole as a white solid, with a yield of 83.6%, and a water content of 0.29%. .

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Abstract

The invention discloses a preparation method of anhydrous dextro lansoprazole. The preparation method comprises the following steps: dissolving or suspending dextro lansoprazole with the water content of 5-15% into a low-boiling-point organic solvent, carrying out reduced pressure concentration to be dry, repeatedly operating for 1-2 times, then adding a low-polarity organic solvent, stirring and pulping at room temperature, and carrying out suction filtration, washing and vacuum drying, thus obtaining the anhydrous dextro lansoprazole with the water content of less than or equal to 0.5%. According to the preparation method disclosed by the invention, the operation is simple and convenient, and the obtained anhydrous dextro lansoprazole has good stability.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, in particular to a preparation method of anhydrous dexlansoprazole. Background technique [0002] Dexlansoprazole is a drug developed and marketed by Takeda Corporation of Japan for the treatment of gastroesophageal reflux. The drug is an enantiomer of the proton pump inhibitor lansoprazole, also known as dexlansoprazole, and is used to treat heartburn and varying degrees of erosive esophagus associated with non-erosive gastroesophageal reflux disease inflammation. [0003] Dexlansoprazole, whose chemical name is (R)-2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridyl]methyl]- Sulfinyl] benzimidazole, its structure is shown in formula (I): [0004] [0005] CN103709139A discloses a preparation method of anhydrous dexlansoprazole, which is obtained by suspending dexlansoprazole hydrate in methyl tert-butyl ether, heating reflux, separating water to separate out solids, or suspending in ether...

Claims

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Application Information

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IPC IPC(8): C07D401/12
CPCC07D401/12C07B2200/07
Inventor 张峰李上朱素华薛峪泉刘春猛
Owner 南京博德生物制药有限公司
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