Preparation method of high-purity esomeprazole sodium salt

A technology of esomeprazole salt and meprazole salt, which is applied in the field of compound salt purification, can solve the problems of high production cost and large amount of solvent, and achieve the effect of simple steps

Active Publication Date: 2013-03-27
科贝源(北京)生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The product purity that this method obtains is relatively high, but solvent consumption is relatively large, a

Method used

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  • Preparation method of high-purity esomeprazole sodium salt
  • Preparation method of high-purity esomeprazole sodium salt
  • Preparation method of high-purity esomeprazole sodium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Take 100 grams of esomeprazole sodium crude product, add 160 grams of methanol, stir and dissolve at 25°C. After dissolving, cool down to 0°C and stir for 2 hours, then filter. After drying the filter cake at 80-85°C for 2 hours, add 200 grams of acetone to the product, add and reflux for 2 hours, and cool to room temperature. Filtrate, and dry the filter cake at 80-85°C for 2 hours to obtain 54 grams of esomeprazole sodium. Checked by HPLC, the single impurity is less than 0.1%, and the purity is greater than 99.7%. Moisture content (Karl Fischer method) 0.31, placed under the condition of relative humidity 80% for 12 hours, water content 3.8%.

[0044] HPLC method:

[0045] Stationary phase: C8 column (4.6×150mm, 5μm)

[0046] Mobile phase: phosphate buffer (weigh 1.4g sodium dihydrogen phosphate pentahydrate into 1000ml water, adjust pH=7.90 with phosphoric acid)-acetonitrile (73:27)

[0047] Detection wavelength: 280nm

[0048] Flow rate: 1.0ml / min

[0049] Inj...

Embodiment 2

[0052] Take 100 grams of esomeprazole sodium crude product, add 160 grams of methanol, stir and dissolve at 20°C. After dissolving, cool down to -5°C and stir for 2 hours, then filter. After drying the filter cake at 80-85°C for 2 hours, add 200 grams of acetone to the product, add and reflux for 2 hours, and cool to room temperature. Filter, and dry the filter cake at 80-85° C. for 2 hours to obtain 62 grams of esomeprazole sodium. Checked by HPLC, the single impurity is less than 0.1%, and the purity is greater than 99.7%. Moisture content (Karl Fischer method) 0.24, placed under the condition of relative humidity 80% for 12 hours, water content 4.3%.

[0053] The HPLC method is the same as in Example 1.

Embodiment 3

[0055] Take 100 grams of esomeprazole sodium crude product, add 300 grams of methanol, stir and dissolve at 30°C. After dissolving, cool down to 0°C and stir for 3 hours, then filter. After drying the filter cake at 80-85°C for 2 hours, add 200 grams of acetonitrile to the product, add and reflux for 3 hours, and cool to room temperature. Filtrate, and dry the filter cake at 80-85° C. for 2 hours to obtain 48 grams of esomeprazole sodium. Checked by HPLC, the single impurity is less than 0.1%, and the purity is greater than 99.7%. Moisture content (Karl Fischer method) 0.31, placed under the condition of relative humidity 80% for 12 hours, water content 3.9%.

[0056] The HPLC method is the same as in Example 1.

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Abstract

The invention provides a refining method of industrial esomeprazole sodium salt. The preparation method is characterized by comprising the following steps: adding esomeprazole sodium salt to methanol, the amount of which is 1.6-4 times of that of the esomeprazole sodium salt; stirring and dissolving the esomeprazole sodium salt under the room temperature; filtering the mixture to obtain a settled solution; cooling the settled solution at 0 DEG C and stirring the settled solution for 2-4 hours; filtering and drying the precipitate; using poor solvents such as acetone, acetonitrile, isopropyl ether and the like for heating and refluxing the mixture for 2-4 hours; cooling the mixture to room temperature, and filtering and drying the mixture. Through the preparation method, high-purity esomeprazole sodium salt can be obtained, single purity content does not exceed 0.1%, the moisture content is smaller than 1%; and the moisture content does not exceed 5% after placing the mixture for 12 hours at 40 DEG C under the relative humidity of 80%.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for purifying compound salts. Background technique [0002] Proton pump inhibitors were discovered in the 1980s and have significantly changed the clinical treatment effects of acid-related diseases such as peptic ulcer, gastroesophageal reflux, and functional dyspepsia. At present, the first-generation proton pump inhibitors commonly used in clinical practice include: omeprazole, lansoprazole, pantoprazole, etc., and the second-generation proton pump inhibitors include: rabeprazole, esomeprazole, These proton pump inhibitors have been clinically applied, have remarkable curative effect, are safe and reliable, and are convenient to take. [0003] Esomeprazole is the left-handed optically pure isomer of omeprazole (the structure is as follows). Compared with omeprazole, the individual differences in its metabolism are smaller, and the clinical treatment effe...

Claims

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Application Information

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IPC IPC(8): C07D401/12
Inventor 郑祖爽梁飞陈振刚
Owner 科贝源(北京)生物医药科技有限公司
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