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Pantoprazole salt crystal form and preparation method thereof

A technology of pantoprazole and pantoprazole potassium, applied in the field of chemical synthesis, can solve problems such as low decomposition temperature, poor thermal stability, etc., and achieves the effects of high active ingredients, reduced requirements for preservation conditions, and easy preservation

Active Publication Date: 2012-10-10
HANGZHOU ZHONGMEI HUADONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In summary, the product obtained by the prior art h

Method used

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  • Pantoprazole salt crystal form and preparation method thereof
  • Pantoprazole salt crystal form and preparation method thereof
  • Pantoprazole salt crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045]Take by weighing 10.84mg potassium hydroxide in the 4mL vial, then weigh 73.4mg of pantoprazole free acid in the vial, add 0.2mL methanol, stir to make the system dissolve, stir at room temperature for 2 hours, and then under vacuum (T =40°C, P=-0.1MPa) by rotary evaporating methanol to dryness, adding 1.5mL anti-solvent MTBE for ultrasonic crystallization, and then concentrating to dry MTBE under reduced pressure to obtain off-white potassium salt.

[0046] X-ray powder diffraction (XRPD): Bruker Advance Bruker D8 diffractometer for X-ray powder diffraction pattern, Ca-Ku ray (40kV, 40mA), θ-2θ goniometer, Mo monochromator and Lynxeye detector, the instrument is in Check and calibrate with emery before use. The acquisition software is Diffrac Plus XRD Commander, and the analysis software is Diffrac Plus EVA / Jade 6.

[0047] Samples were tested at room temperature. Put the sample to be tested on the plexiglass slide. Samples were not ground before testing. See below ...

example example 2

[0055] Example 2, crystallization test

[0056] Weigh 441mg of potassium hydroxide into a 50mL one-necked bottle, then accurately weigh 2011mg of free acid into a one-necked bottle, add 50mL of methanol, stir to dissolve the system, stir at room temperature for 20 hours, and then under vacuum (T=40℃, P=-0.09MPa) Rotatingly evaporate methanol to dryness, add anti-solvent MTBE 80mL for ultrasonic crystallization, and then concentrate under reduced pressure to dry MTBE to obtain off-white potassium salt.

[0057] Using the equipment and method described in Example 1, XRD characterization, it is found that the crystal form is the same as that in Example 1.

[0058]

example example 3

[0059] Example 3, scale-up test

[0060] Weigh 1.6kg of potassium hydroxide in a 250L reaction bottle, then weigh 10 kg of free acid into the reaction bottle, add 80L of methanol, stir to dissolve the system, stir at room temperature for 8 hours, and then under vacuum (T=40℃ , P=-0.08MPa) Rotary evaporated methanol to dryness, added anti-solvent MTBE 300L for ultrasonic crystallization, and then concentrated under reduced pressure to dry MTBE to obtain off-white potassium salt.

[0061] Using the equipment and method described in Example 1, XRD characterization, it is found that the crystal form is the same as that in Example 1.

[0062]

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Abstract

The invention provides a new pantoprazole salt crystal form which can radiate by use of Cu-Ka, and is characterized in that in the X-ray powder diffraction pattern, the angle 2 theta represented by degrees has characteristic diffraction peaks at the parts about 5.97, 12.53, 12.93, 14.85, 15.85, 16.42, 18.00, 20.34, 21.30, 22.02, 22.58, 23.86, 24.91, 26.99, 28.43, 29.09, 30..50, 33.30 and 35.00 degrees. The pantoprazole salt crystal form provided by the invention is high in decomposition temperature and good in stability. The invention also provides a method which is used for preparing the pantoprazole salt crystal form and is easy in industrialization, and a compound containing the pantoprazole salt crystal form.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a crystal form of pantoprazole salt and a preparation method thereof. Background technique [0002] Pantoprazole (Pantoprazole), its chemical name is: 5-difluoromethoxy-2-[(3,4-dimethoxy-2-pyridyl)methyl]sulfinyl-1H-benzo Imidazole is a proton pump inhibitor antiulcer drug. [0003] Pantoprazole sodium salt is currently widely used clinically for the treatment of peptic ulcer bleeding, acute gastric mucosal injury caused by non-steroidal anti-inflammatory drugs, ulcer bleeding under stress, general anesthesia or major surgery Prevention of gastric acid reflux combined with aspiration pneumonia and other diseases in debilitated and comatose patients. [0004] Pantoprazole potassium has the same pharmacological action as pantoprazole sodium. However, there are few studies on potassium salt at present. [0005] The decomposition temperature of the product is an import...

Claims

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Application Information

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IPC IPC(8): C07D401/12A61K31/4439A61P1/04
Inventor 徐仲军谢厅
Owner HANGZHOU ZHONGMEI HUADONG PHARMA
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