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Separation and purification method of lansoprazole intermediate 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine

A technology of trifluoroethoxy and lansoprazole, which is applied in the field of separation and purification of pharmaceutical intermediates, can solve problems such as poor separation and purification effects, achieve high market value, high purity of finished products, and improve the effect of separation and purification

Active Publication Date: 2018-05-18
FUZHOU SANHE PHARMACHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the defect of poor separation and purification effect of lansoprazole intermediate 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine in the prior art, Lansoprazole is provided Separation and purification method of 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine, an intermediate of prazole

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The separation and purification method of lansoprazole intermediate 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine comprises the following steps:

[0020] The crude 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine was heated and sublimated under reduced pressure, and the vaporized 2-hydroxymethyl-3-methyl- 4-(2,2,2-trifluoroethoxy)pyridine was cooled and sublimated to obtain 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine for one-time separation and purification product, add the obtained 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine to the solvent for one-time separation and purification, stir and mix well, and then add the decolorizing The decolorizing agent is heated and stirred while hot to remove the decolorant, the obtained filtrate is cooled and recrystallized, the crystals are collected by filtration, and the crystals are heated and dried to obtain 2-hydroxymethyl-3-methyl-4-(2,2, 2-trifluoroethoxy)pyridine finished ...

Embodiment 2

[0024] The separation and purification method of lansoprazole intermediate 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine comprises the following steps:

[0025] The crude product of 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine is heated and sublimated under reduced pressure, which means that the sublimation process starts at Under normal pressure, start the vacuum pump to reduce the pressure to 5 mmHg, and the heating temperature for heating and sublimation under reduced pressure is 130 degrees Celsius.

[0026] The vaporized 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine is cooled and sublimated to obtain 2-hydroxymethyl-3-methyl-4-(2, 2,2-trifluoroethoxy)pyridine primary separation and purification product, the obtained 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine primary separation and purification product After adding into the solvent, stirring and mixing, adding a decolorizing agent into the solvent, heating and stirri...

Embodiment 3

[0031] The separation and purification method of lansoprazole intermediate 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine comprises the following steps:

[0032]The crude 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine was heated and sublimated under reduced pressure, and the vaporized 2-hydroxymethyl-3-methyl- 4-(2,2,2-trifluoroethoxy)pyridine was cooled and sublimated to obtain 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine for one-time separation and purification product, add the obtained 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine to the solvent for one-time separation and purification, stir and mix well, and then add the decolorizing The decolorizing agent is heated and stirred while hot to remove the decolorant, the obtained filtrate is cooled and recrystallized, the crystals are collected by filtration, and the crystals are heated and dried to obtain 2-hydroxymethyl-3-methyl-4-(2,2, 2-trifluoroethoxy)pyridine finished p...

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Abstract

The invention discloses a separation purification method of a lansoprazole intermediate 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine, which comprises the following steps: heating a crude product under normal pressure or reduced pressure for sublimation, cooling the gasification product for desublimation to obtain a 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine primary separation purification product, adding into a solvent, evenly mixing, adding a decolorant into the solvent, heating while stirring, filtering out the decolorant while the solution is hot, cooling the obtained filtrate to recrystallize, filtering to obtain the crystal, and drying the crystal by heating to obtain the finished product. The reduced pressure sublimation process is adopted to perform sublimation treatment on the 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine crude product to obtain the product with favorable color, and the purity of the product is up to 99.8% above.

Description

technical field [0001] The invention relates to the field of separation and purification methods of pharmaceutical intermediates, especially the separation and purification of lansoprazole intermediate 2-hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine method. Background technique [0002] Lansoprazole (Lansoprazole) is the second proton pump inhibitor after Omeprazole (Omeprazole), developed by Takeda Corporation of Japan, and was first launched in France in 1991. It inhibits the proton pump of the parietal cells of the gastric mucosa, that is, the activity of H+ / K+2ATPase, continuously and effectively inhibits the secretion of gastric acid, and is effective for gastric, duodenal ulcer, anastomotic ulcer, reflux esophagitis and Zol-Ellard syndrome has a good therapeutic effect. 2-Hydroxymethyl-3-methyl-4-(2,2,2-trifluoroethoxy)pyridine is an important intermediate for the synthesis of lansoprazole, and the existing synthetic method obtains 2-hydroxymethyl The cru...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/68
CPCC07D213/68
Inventor 陈英奇程杰兵俞农赵军
Owner FUZHOU SANHE PHARMACHEM