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Purification method of crude product of desloratadine

A technique for desloratadine and a purification method, which is applied in the field of purification of crude desloratadine, can solve the problems of large product loss, long time consumption, and many impurities in the crude product, and achieve high product yield, shortened time, The effect of simple process

Inactive Publication Date: 2018-08-03
CHANGZHOU FANGYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Usually, desloratadine is prepared by the hydrolysis reaction of loratadine in an aqueous solution of alkaline ethanol, and this reaction usually requires heating and reflux for a long time (such as patent document WO2004029039), and the resulting desloratadine The crude product has many impurities, and this crude product can reach a purity of 95 to 98% after the post-treatment of the recrystallization method recorded in the prior art, but the product loss is relatively large and the yield is small
Although the preparation method described in the patent document CN104961724B and the desloratadine crude product (the desloratadine-containing feed liquid obtained after the reaction) post-treatment method obtain higher purity and higher yield, the post-treatment consumes The longer the time, the more waste water will be generated

Method used

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  • Purification method of crude product of desloratadine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 10 g of crude desloratadine into a 500 mL eggplant-shaped bottle, and add acetone-tetrahydrofuran (5:1) mixed solvent under heating at 40°C until the crude product is completely dissolved. Stop heating, let stand for crystallization overnight. Filter to get 8.9g desloratadine. HPLC analysis showed that the impurity content was 0.04%.

Embodiment 2

[0041] S10, at 40 DEG C, 10g desloratadine crude product is dissolved in the mixed solvent of 30mL ketone organic solvent and cyclic ether organic solvent; Wherein the volume ratio of ketone organic solvent and cyclic ether organic solvent is 4: 1;

[0042] S11, cooling to -6°C, filtering to obtain solid a and filtrate a;

[0043] S12. Heat the filtrate a to 40°C, stir for 20 minutes, cool down to -6°C, and filter to obtain solid b and filtrate b;

[0044] S13. At 40°C, solid a and solid b are combined and dissolved again with a mixed solvent of ketone organic solvent and cyclic ether / ester organic solvent;

[0045] S20. Naturally cool down to room temperature 20° C., precipitate crystal a, and filter the precipitated crystal a to obtain pure desloratadine.

[0046] Result: due to the low-temperature crystallization in steps S11~S12, the solid precipitation time is short, and the time required for crystallization in steps S11~S12 and step S20 is less than 3h, without overnig...

Embodiment 3

[0048] S10. Dissolve 100 g of crude desloratadine in 400 mL of a mixed solvent of ketone organic solvents and ester organic solvents at 50° C.; wherein the volume ratio of ketone organic solvents to cyclic ether organic solvents is 4:1 ;

[0049] S11, cooling to -3°C, filtering to obtain solid a and filtrate a;

[0050] S12. Warm up the filtrate a to 50°C, stir for 20 minutes, cool down to -3°C, and filter to obtain solid b and filtrate b;

[0051] S13. At 50°C, solid a and solid b are combined and dissolved again with a mixed solvent of ketone organic solvent and cyclic ether / ester organic solvent;

[0052] S20, cooling in an ice-water bath to precipitate crystal a, and filter the precipitated crystal a to obtain pure desloratadine.

[0053] Results: Due to the low-temperature crystallization in steps S11~S12, the time for solid precipitation is short, and the time required for crystallization in steps S11~S12 and step S20 is less than 5 hours, without overnight, the time f...

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Abstract

The invention discloses a purification method of a crude product of desloratadine. The purification method is characterized by comprising the following steps that S10, the crude product of desloratadine is dissolved in a mixed solvent of a ketone organic solvent and a cyclic ether / ester organic solvent at a first preset temperature; and S20, a crystal a is separated out at a second preset temperature, the crystal a is filtered and separated out, the a purified product of desloratadine is obtained, and the second preset temperature is lower than the first preset temperature. The method is simple in technology, the post-purification time is shortened, the using amount of the organic mixed solvent for crystallization is less, a larger amount of waste liquid cannot be generated, the purity ofthe obtained purified product of desloratadine is high, and the product yield rate is high.

Description

technical field [0001] The present invention relates to a kind of medicine purification method, more specifically, relate to a kind of desloratadine crude product purification method. Background technique [0002] Desloratadine is the active metabolite of loratadine, which is a white or off-white solid, and its structural formula is: [0003] [0004] Desloratadine is a non-sedating long-acting tricyclic antihistamine drug, which can relieve symptoms related to allergic rhinitis or chronic idiopathic urticaria. It has strong effect and good safety. Usually, desloratadine is prepared by the hydrolysis reaction of loratadine in an aqueous solution of alkaline ethanol, and this reaction usually requires heating and reflux for a long time (such as patent document WO2004029039), and the resulting desloratadine The crude product has many impurities, and this crude product can reach a purity of 95% to 98% after the post-treatment of the recrystallization method recorded in the ...

Claims

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Application Information

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IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 李红杰印靖王海东戴俊戚斌
Owner CHANGZHOU FANGYUAN PHARMA
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