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Preparation method of escomeprazole magnesium dihydrate crystal with high crystal form purity

A technology of magnesium azole dihydrate and magnesium azole trihydrate, which is applied in the field of medicinal chemistry, can solve the problems of difficulty in preparing drugs with crystal form purity, wide particle size distribution, poor fluidity, etc., and achieve saving manpower and material resources, qualified magnesium content, The effect of short crystallization time

Active Publication Date: 2022-04-12
SHOUGUANG FUKANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For esomeprazole magnesium, there are many drug crystals, the common ones are esomeprazole magnesium anhydrate, esomeprazole magnesium dihydrate crystal form A, esomeprazole magnesium Meprazole magnesium dihydrate crystal form B, esomeprazole magnesium trihydrate, etc., wherein, esomeprazole magnesium dihydrate crystal form A has higher efficacy, but at present, the preparation of esmeprazole magnesium Omeprazole magnesium dihydrate crystal form A technology has limitations, it is difficult to prepare esomeprazole magnesium dihydrate crystal form A solid drug with high crystal form purity, in addition, currently, esomeprazole magnesium There are still technical problems in the preparation process of the dihydrate crystal form A drug, such as wide particle size distribution, poor fluidity, and high magnesium content.

Method used

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  • Preparation method of escomeprazole magnesium dihydrate crystal with high crystal form purity
  • Preparation method of escomeprazole magnesium dihydrate crystal with high crystal form purity
  • Preparation method of escomeprazole magnesium dihydrate crystal with high crystal form purity

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Embodiment 1

[0029] A method for preparing esomeprazole magnesium dihydrate crystals with high crystalline purity using esomeprazole magnesium trihydrate as a raw material, specifically:

[0030] 1. Dissolving and concentrating: Firstly, at 25°C, dissolve 10g of esomeprazole magnesium trihydrate in 150mL of methanol, and filter after the dissolution is complete to obtain a methanol solution of esomeprazole magnesium; The methanol solution of someprazole magnesium is evaporated under reduced pressure, and the temperature of controlling the evaporated under reduced pressure is 35° C., and the pressure of evaporated under reduced pressure is -0.09 MPa. When the residual amount of the solution is 50 g, the evaporation is stopped to obtain the mother liquor, and the mother liquor is transferred to 250 mL jacketed crystallizer.

[0031] 2. Adding eluent and crystallization dropwise: Mix 100 mL of acetone and 10 mL of water evenly, then ultrasonically mix for 10 min, and pass through a 0.45 micro...

Embodiment 2

[0038] A method for preparing esomeprazole magnesium dihydrate crystals with high crystal purity by using esomeprazole magnesium dihydrate crystal form B as a raw material, specifically:

[0039] 1. Suspension and crystallization: Mix 100 mL acetone and 10 mL water evenly, then ultrasonically mix for 10 min, and pass through a 0.45 micron membrane to obtain the eluent;

[0040] 10g of esomeprazole magnesium dihydrate crystal form B solid was added to the dissolution agent to obtain a suspension, and the suspension was added to a 250 mL jacketed crystallizer, and the temperature of the 250 mL jacketed crystallizer was set to 15°C and start stirring to perform suspension crystallization, control the stirring speed to 350rpm, control the suspension crystallization time to 6h, filter after the suspension crystallization is completed, and rinse with acetone to obtain the transition state crystal form of esomeprazole magnesium hydrate, which The water content is 12%.

[0041]2. dry...

Embodiment 3

[0043] A method for preparing esomeprazole magnesium dihydrate crystals with high crystalline purity using esomeprazole magnesium trihydrate as a raw material, specifically:

[0044] 1. Dissolving and concentrating: Firstly, at 15°C, dissolve 10g of esomeprazole magnesium trihydrate in 150mL of methanol, and filter after dissolving completely to obtain a methanol solution of esomeprazole magnesium; The methanol solution of someprazole magnesium is evaporated under reduced pressure, and the temperature of controlling the evaporated under reduced pressure is 35 ℃, and the pressure of evaporated under reduced pressure is -0.06MPa, and when the remaining amount of the solution is 50g, the evaporation is stopped to obtain the mother liquor, and the mother liquor is transferred to 250 mL jacketed crystallizer.

[0045] 2. Adding eluent and crystallization dropwise: Mix 100 mL of acetone and 10 mL of water evenly, then ultrasonically mix for 10 min, and pass through a 0.45 micron mem...

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Abstract

The invention discloses a preparation method of a high-crystal-form-purity escomeprazole magnesium dihydrate crystal, and belongs to the technical field of medical chemistry, and the preparation method comprises the following steps: dropwise adding a solventing-out agent, performing crystal transformation, drying and controlling the water content; the step of dropwise adding the solvating-out agent and performing crystal transformation comprises the following steps: controlling the temperature of the escomeprazole magnesium intermediate to be 15-25 DEG C, adding the solvating-out agent while stirring, performing crystal transformation at-5-20 DEG C, controlling the crystal transformation time to be 4-8 hours, and obtaining an escomeprazole magnesium hydrate in a transition-state crystal form after crystal transformation is finished; in the drying and water content control step, the escomeprazole magnesium hydrate in the transition-state crystal form is dried; the escomeprazole magnesium dihydrate crystal prepared by the preparation method is high in crystal form purity, narrow in particle size distribution, good in fluidity and low in magnesium content.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a preparation method of esomeprazole magnesium dihydrate crystal with high crystal form purity. Background technique [0002] Esomeprazole magnesium is the S-isomer of omeprazole, which is weakly alkaline, concentrates and converts into the active form in the high-acid environment of the acid-oxyntic microtubules of the parietal cells, and inhibits the H+– K+–ATPase (proton pump), which in turn inhibits both gastric acid and stimulation-induced gastric acid secretion. It is characterized by a small hepatic first-pass effect after oral administration, and higher bioavailability and plasma concentration than omeprazole or the R-isomer. Therefore, its drug effect is higher and longer-lasting than that of omeprazole. [0003] For esomeprazole magnesium, there are many drug crystals, the common ones are esomeprazole magnesium anhydrate, esomeprazole magnesium dihydrate cr...

Claims

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Application Information

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IPC IPC(8): C07D401/12
Inventor 薛富民李洪程于帅刘彬王艳国建辉杜世超董良军高东圣褚亚飞
Owner SHOUGUANG FUKANG PHARMA
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