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Loratadine compound and preparation method thereof

A technology of loratadine and compounds, applied in the field of loratadine compounds and its purification process, can solve the problems of reduced yield of purified products or intermediates, low purity of target products, less purity can be obtained, etc. Achieve the effects of easy control and industrialized production, low cost, and reduced toxic and side effects

Inactive Publication Date: 2012-02-01
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The syntheses described so far thus involve various disadvantages, including a high number of steps, use of reagents which are difficult to handle on an industrial level, generation of unwanted side reaction products, and consequently reactions to purify products or intermediates with reduced yields
[0011] These methods can effectively prepare loratadine, but the unavoidable problem is that the purity of the target product is not high, and the product post-treatment or purification method provided is a conventional method in organic chemical synthesis, and these methods are rarely able to obtain 95% or Purity above

Method used

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  • Loratadine compound and preparation method thereof
  • Loratadine compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Dissolve 10g of crude loratadine with a purity of 94.8% in 100ml of isopropanol, then add 0.1g of activated carbon, heat and stir at 30°C for 10 minutes, and filter to obtain primary purified loratadine; After the solution is concentrated, add 10g of pretreated DA-201 type macroporous adsorption tree, stir and mix well, add to the top of DA-201 type macroporous adsorption resin column, first wash with 1-2 column volumes of purified water until it is clear , And then eluted with 50% isopropanol containing 0.01mol / L hydrochloric acid, collected the eluate, concentrated under reduced pressure to about two-fifths of the volume to obtain secondary purified loratadine; stirred at 50-60°C Next, add ammonia water to the concentrated solution to pH 8.0, cool to 0~4°C overnight, separate out crystals, centrifuge, wash, and dry to obtain 9.07 g of three-stage purified loratadine with a purity of 99.63% and a yield of 95.70 %. MP: 135~136℃

Embodiment 2

[0043] Dissolve 10g of crude loratadine with a purity of 94.8% in 100ml of isopropanol, then add 0.3g of activated carbon, heat and stir at 40°C for 15 minutes, and filter to obtain primary purified loratadine; After the solution is concentrated, add 10g of the pretreated Diaion HP2MG type macroporous adsorption tree, stir and mix well, add to the top of the Diaion HP2MG type macroporous adsorption resin column, first wash with 1 to 2 column volumes of purified water until it is clear, then Elute with 50% isopropanol containing 0.01mol / L hydrochloric acid, collect the eluate, concentrate under reduced pressure to about two-fifths of the volume to obtain secondary purified loratadine; Ammonia water was added to the concentrated solution to pH 8.2, cooled to 0-4°C overnight, crystals were precipitated, centrifuged, washed, and dried to obtain 9.03 g of three-stage purified loratadine with a purity of 99.75% and a yield of 95.28%. MP: 135~136℃.

Embodiment 3

[0045] Dissolve 10g of crude loratadine with a purity of 94.8% in 100ml of isopropanol, then add 0.4g of activated carbon, heat and stir at 50°C for 20 minutes, and filter to obtain primary purified loratadine; After the solution is concentrated, add 10g of pretreated AB-8 type macroporous adsorption tree, stir and mix well, add to the top of the AB-8 type macroporous adsorption resin column, first wash with 1 to 2 column volumes of purified water until it is clear , And then eluted with 50% isopropanol containing 0.01mol / L hydrochloric acid, collected the eluate, concentrated under reduced pressure to about two-fifths of the volume to obtain secondary purified loratadine; stirred at 50-60°C Add ammonia water to the concentrated solution until the pH value is 8.5, cool to 0~4℃ overnight, precipitate crystals, centrifuge, wash, and dry to obtain 8.99 g of three-stage purified loratadine with a purity of 99.87% and a yield of 94.8 %. MP: 135~136℃.

[0046] The following lists som...

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Abstract

The invention relates to a method for preparing a loratadine compound. The method comprises the following steps of: (1) dissolving crude loratadine into an appropriate organic solvent, adding active carbon for adsorbing, heating, stirring, and filtering to obtain primarily-purified loratadine; (2) concentrating the solution, loading onto a macroporous absorption resin column, washing to clear state with purified water, eluting with 50 percent isopropyl alcohol containing 0.01 mol / L HCl, and collecting an eluent to obtain secondarily-purified loratadine; and (3) adjusting the pH of the eluent with an alkaline solution, cooling for crystalizing, centrifuging the separated crystal, washing and drying to obtain trebly-purified loratadine. The purity of fine loratadine obtained with the method is not less than 99.5 percent, the quantity of ignition residues is extremely small, and the heavy metal content is extremely low. The method has the characteristics of easiness, convenience and easiness for controlling and industrial production; and simultaneously, the toxic and side effects of the loratadine compound which is taken as an antihistamine medicament are reduced, and the preparation product quality is improved.

Description

Technical field [0001] The invention relates to a loratadine compound and its purification process, and belongs to the technical field of medicine. Background technique [0002] Loratadine (Loratadine), the chemical name is: 4-(8-chloro-5,6-dihydro-11H-benzo5,6-cycloheptano1,2-bpyridine-11-subunit)-1 -Ethyl piperidine carboxylate, molecular formula: C 22 H 23 ClN 2 O 2 , Molecular weight: 382.89, structural formula: [0003] [0004] Loratadine is a non-sedative, long-acting tricyclic antihistamine developed by Schering-Plough. It has selective anti-peripheral H1 receptor effect. It was first developed by Schering-Plough in 1988. Launched in Belgium, as a third-generation antihistamine, it has the characteristics of fast onset and strong action. Studies with guinea pigs have shown that the action time of this product is 18-24 hours. Research on the central function shows that this product has little or no inhibitory or anticholinergic effect on mice, rats, dogs and monkeys. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04A61P37/08
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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