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A kind of preparation method of high-purity esomeprazole sodium

A technology of esomeprazole sodium and omeprazole sodium salt, which is applied in the field of preparation of high-purity esomeprazole sodium, and can solve the difficulty of splitting titanium complex suspensions and the ammonia complexation of titanium Problems such as difficult to remove, to achieve the effect of low production cost, high product purity and high yield

Active Publication Date: 2016-01-20
SICHUAN BAILI PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide an industrialized high-purity Angstrom The preparation method of Someprazole Sodium

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: a kind of preparation method of high-purity esomeprazole sodium comprises the following steps:

[0032] Add 0.5L of water into 160L of n-propanol, add 10kg of omeprazole sodium under stirring, stir until the solution is clear, then add 4.6L of D-(-)-diethyl tartrate and 4.05L of tetraisopropoxytitanium in sequence , 11.3L of triethylamine, 6.13kg of L-(+)-mandelic acid, reacted at 40°C for 3.5h, and filtered to obtain a white solid.

[0033] Add the white solid and 60L saturated aqueous sodium bicarbonate solution to 60L ethyl acetate, stir for 0.5h, back-extract the aqueous layer once with 20L ethyl acetate, combine the ethyl acetate layers and sequentially wash with saturated aqueous sodium bicarbonate solution 15L*2, 10L Wash with water; collect the ethyl acetate layer, add 40L of 12.5% ​​ammonia water, stir for 20min, stand for liquid separation, wash the ethyl acetate layer with 10Lx2 of 12.5% ​​ammonia water, combine the ammonia water layer; add the ...

Embodiment 2

[0035] Embodiment 2: a kind of preparation method of high-purity esomeprazole sodium comprises the following steps:

[0036]Add 0.5L of water to 150L of n-propanol, add 10kg of omeprazole sodium while stirring, stir until the solution is clear, then add 4.6L of D-(-)-diethyl tartrate and 4.05L of tetraisopropoxytitanium in sequence , 11.3L of triethylamine, 6.13kg of L-(+)-mandelic acid, reacted at 40°C for 3.5h, and filtered to obtain a white solid.

[0037] Add the white solid and 60L saturated aqueous sodium bicarbonate solution to 60L ethyl acetate, stir for 0.5h, back-extract the aqueous layer once with 20L ethyl acetate, combine the ethyl acetate layers and sequentially wash with saturated aqueous sodium bicarbonate solution 15L*2, 10L Wash with water; collect the ethyl acetate layer, add 40L of 12.5% ​​ammonia water, stir for 20min, stand for liquid separation, wash the ethyl acetate layer with 10Lx2 of 12.5% ​​ammonia water, combine the ammonia water layer; add the amm...

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Abstract

The invention discloses a preparation method for high-purity esomeprazole sodium. The preparation method comprises the steps of: including and splitting esomeprazole sodium and D-(-)-diethyl tartrate, titanium iso-propylate, triethylamine and L-(+)-mandelic acid in the presence of a proper amount of water, and separating to obtain an inclusion complex; dissolving the inclusion complex with ethyl acetate, washing inclusion complex with sodium carbonate water solution, carrying out ammonia hydroxide eluting on an ethyl acetate layer, slowly regulating the pH value to 6-7 with glacial acetic acid, then extracting with dichloromethane, and concentrating to obtain crude esomeprazole free alkali product; carrying out silica gel adsorption and elution on the crude product to obtain a pure esomeprazole free alkali product; and enabling the pure product and the methanol-ethanol-acetonitrile solution of sodium hydroxide to form salt, and then crystallizing with isopropyl ether to obtain the high-purity esomeprazole sodium. According to the preparation method, the difficulties that when inclusion and splitting are carried out, the titanium complex suspension body are difficult to split and the ammonia complex of titanium is difficult to remove can be solved, the industrialization production can be realized, the industrialized production cost is low, the product purity is high, the yield is high, and no harmful gas is generated.

Description

technical field [0001] The invention belongs to the technical field of chemical pharmacy and relates to a preparation method of high-purity esomeprazole sodium. Background technique [0002] Esomeprazole sodium (Esomeprazolesodium, C 17 h 18 N 3 NaO 3 S), the S-optical isomer of omeprazole, is the world's first isomer proton pump inhibitor (PPI), which reduces gastric acid secretion by specifically inhibiting the proton pump of gastric parietal cells. A large number of clinical experiments and drug studies have confirmed that it can maintain gastric pH>4 for a longer time, have higher acid suppression efficiency, and have better curative effect than the previous two generations of PPI, with little individual difference. As a new generation of PPI, it has been widely used in clinical treatment of many acid-related diseases. [0003] Inclusion resolution is a chiral drug resolution method developed in this year. During its production, it is easy to produce titanium com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/12
Inventor 朱义吴勇王一茜
Owner SICHUAN BAILI PHARM CO LTD
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