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Preparation method of high-purity small-particle-size pranlukast

A small particle size, high purity technology, applied in organic chemistry and other directions, can solve the problems of poor solvent heating and reflux, difficult to meet particle size requirements, poor purification effect, etc., and achieve the effect of crystallization process block, easy pulverization, and simple operation.

Pending Publication Date: 2021-11-09
HUNAN FURUI BIOPHARMA TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In his master's thesis, Shi Gang described the method of heating and refluxing with a poor solvent for purification. The purification effect of a single solvent is poor, while the purification effect of a mixed solvent is better. Ethanol / dimethylformamide, methanol / dimethylformamide are preferred. Dimethyl formamide and ethyl acetate / dimethyl formamide have better effects. Repeating the above experiments, the researchers found that after one purification of the mixed solvent, the purity of the product can reach 99.0%. To further improve the purity, multiple refinements are required; research The personnel also found that the granules prepared after purification have a large particle size, and it is still difficult to meet the particle size requirement of particle size distribution D90≤20μm after repeated crushing

Method used

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  • Preparation method of high-purity small-particle-size pranlukast

Examples

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Effect test

Embodiment 1

[0022] Example 1: In the mixed solvent of 400g ethyl acetate and 600g dimethylformamide, add 400g of pranlukast crude product (purity 95.4%), start stirring, heat up to slight reflux, after completely dissolving, in stirring state , the above solution was added to 1000mL aqueous sodium bicarbonate solution (concentration 10% m / m) at 0°C, a solid was precipitated under rapid stirring, filtered, the filter cake was washed with purified water, and the solid was vacuum-dried. The particle size distribution D90 is 58.5 μm, and the product purity is 99.6%.

[0023] The above-mentioned pranlukast refined product was pulverized once by jet, and the particle size distribution D90 of the obtained solid powder was 19.2 μm.

Embodiment 2

[0024] Embodiment 2: In the mixed solvent of 100g dichloromethane, 300g ethyl acetate and 600g dimethylformamide, add 400g pranlukast crude product (purity 95.4%), start stirring, heat up to slight reflux, until completely dissolved Finally, under stirring, the above solution was added to 1000ml aqueous sodium bicarbonate solution (concentration 15% m / m) at 0°C, solid was precipitated under rapid stirring, filtered, the filter cake was washed with purified water, and the solid was dried in vacuo. The particle size distribution D90 is 54.3 μm, and the product purity is 99.7%.

[0025] The above-mentioned pranlukast refined product was pulverized once by airflow, and the particle size distribution D90 of the obtained solid powder was 18.1 μm.

Embodiment 3

[0026] Example 3: In the mixed solvent of 300g ethyl acetate and 700g dimethylformamide, add 400g pranlukast crude product (purity 95.4%), start stirring, heat up to slight reflux, after completely dissolving, in stirring state Next, the above solution was added to 1000mL aqueous sodium bicarbonate solution (concentration 10% m / m) at 5°C, solids were precipitated under rapid stirring, filtered, the filter cake was washed with purified water, and the solids were vacuum-dried. The particle size distribution D90 is 57.6 μm, and the product purity is 99.5%.

[0027] The above-mentioned pranlukast refined product was pulverized once by jet, and the particle size distribution D90 of the obtained solid powder was 19.4 μm.

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Abstract

The invention provides a preparation method of high-purity small-particle-size pranlukast. The method comprises the following steps: 1, mixing and dissolving a water-insoluble organic solvent and dimethylformamide, adding a pranlukast crude product, and heating and refluxing to obtain a solution A; 2, quickly adding the solution A into an aqueous solution, and separating out a solid under quick stirring; 3, filtering, separating, drying and sieving to obtain pranlukast with the particle size distribution smaller than 60 microns; and 4, performing primary air jet pulverization on the pranlukast particles with the particle size distribution smaller than 60 microns to obtain pranlukast particles with the particle size distribution D90 smaller than or equal to 20 microns. According to the invention, the pranlukast product with the purity and the particle size meeting the requirements of raw material medicines is prepared at a time, the method is easy to operate, the crystallization process is fast, and the obtained product is easy to smash and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of synthetic pharmacy, in particular to a method for preparing prankast with high purity and small particle size. Background technique [0002] Prankast is a new type of anti-asthma drug launched in the mid-1990s. It is characterized by extremely low toxicity. It is one of the three leukotriene receptor antagonists that are widely concerned in the world. , can significantly inhibit LTC4, LTD4, and LTE4, especially for LTD4 (the main component that causes the contraction of human tracheal smooth muscle). It is effective for chronic, paroxysmal and non-seasonal bronchial asthma; there is no serious adverse reaction, does not affect p450 drug enzyme, and has no drug interaction problem. [0003] It can be found in the existing literature that pranlukast has two solid forms, hemihydrate and anhydrate, wherein the hemihydrate is a stable state, and the anhydrate will rapidly transform into a hemihydrate when the...

Claims

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Application Information

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IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 鲁光英
Owner HUNAN FURUI BIOPHARMA TECH CO LTD
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