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Ibuprofen splitting technology and purifying method based on splitting technology

A purification method and process technology, which is applied in the field of medicine, can solve problems such as complex processes and increased production costs, and achieve the effect of simple split steps, reduced split costs, and simple and environmentally friendly processes

Inactive Publication Date: 2018-04-24
潍坊新益制药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above techniques are comparatively complicated and also increase the production cost. Therefore, developing a new ibuprofen resolution and purification method not only has urgent research value, but also has good economic benefit and industrial application potential. This is exactly the method of the present invention. The driving force and basis for the completion

Method used

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  • Ibuprofen splitting technology and purifying method based on splitting technology
  • Ibuprofen splitting technology and purifying method based on splitting technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] A kind of ibuprofen splitting process, the steps are:

[0054] (1) under normal pressure and condensing condition, 10.3g swirl ibuprofen and ethanol (the feeding ratio of ethanol and swirl ibuprofen is 3ml / g) joins the reaction bottle that is equipped with constant pressure funnel and condensing tube After dissolving, it is heated to 55°C, and R-methylbenzylamine ethanol solution is added dropwise to form a suspension. The ratio of R-methylbenzylamine and dextrin ibuprofen is 0.55:1, wherein R-methylbenzylamine Both methylbenzylamine and dextrin ibuprofen are in moles, and the organic solution of R-methylbenzylamine adopts R-methylbenzylamine ethanol solution, and in the R-methylbenzylamine ethanol solution, R-methylbenzylamine The feed ratio of amine to ethanol is 1:2.5-3.5, wherein R-methylbenzylamine is measured in g, and ethanol is measured in ml;

[0055] (2) Stir the suspension obtained in step (1) for 1 h while maintaining the temperature of step (1);

[0056] ...

Embodiment 2

[0059] A kind of ibuprofen splitting process, the steps are:

[0060] (1) under normal pressure and condensing condition, 10.3g swirl ibuprofen and isopropanol (the feeding ratio of isopropanol and swirl ibuprofen is 3ml / g) join into the constant pressure funnel and condensate In the reaction bottle of tube, after dissolving, be heated to 82 ℃, drop R-methylbenzylamine isopropanol solution, form suspension, the feeding ratio of described R-methylbenzylamine and dextrin ibuprofen is 0.55: 1, wherein R-methylbenzylamine and dextrin ibuprofen are all in moles, and the R-methylbenzylamine organic solution adopts R-methylbenzylamine isopropanol solution, and the R-methylbenzylamine The feed ratio of R-methylbenzylamine and isopropanol in the isopropanol solution is 1:3.5, wherein R-methylbenzylamine is measured in g, and isopropanol is measured in ml;

[0061] (2) Stir the suspension obtained in step (1) for 1 h while maintaining the temperature of step (1);

[0062] (3) After st...

Embodiment 3

[0065] A kind of ibuprofen splitting process, the steps are:

[0066] (1) under normal pressure and condensing condition, 10.3g swirl ibuprofen and isopropanol (the feeding ratio of isopropanol and swirl ibuprofen is 10ml / g) join into the constant pressure funnel and condensate In the reaction bottle of tube, after dissolving, be heated to 82 ℃, dropwise add R-methylbenzylamine isopropanol solution, form suspension, the feeding ratio of described R-methylbenzylamine and dextrin ibuprofen is 0.65: 1, wherein R-methylbenzylamine and dextrin ibuprofen are all in moles, and the R-methylbenzylamine organic solution adopts R-methylbenzylamine isopropanol solution, and the R-methylbenzylamine The feed ratio of R-methylbenzylamine and isopropanol in the isopropanol solution is 1:2.5-3.5, wherein R-methylbenzylamine is in g and isopropanol is in ml;

[0067] (2) Stir the suspension obtained in step (1) for 1 h while maintaining the temperature of step (1);

[0068] (3) After the stir...

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Abstract

The invention discloses an ibuprofen splitting technology and a purifying method based on the splitting technology. The splitting technology comprises the following steps: (1) under the normal pressure and condensation condition, adding mixed suspension ibuprofen into an organic solvent to be heated and dissolved and dropwise adding an R-methylbenzylamine organic solution to form suspension liquid; (2) stirring the suspension liquid obtained in the step (1) for 1 to 3h under the thermal-insulation condition; (3) after stirring, slowly cooling, filtering to remove insoluble salt, concentratingfiltrate to obtain white solid which is an S-ibuprofen crude product obtained by splitting. The ibuprofen splitting technology disclosed by the invention has simple splitting steps, shortens mixed-suspension ibuprofen splitting time, reduces mixed-suspension ibuprofen splitting cost and is easy to achieve industrialization.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a resolution process of ibuprofen and a purification method based on the resolution process. Background technique [0002] Ibuprofen is a non-steroidal anti-inflammatory analgesic, which has analgesic and antipyretic effects, and can relieve rheumatoid arthritis and osteoarthritis. For a long time, it has been sold in racemic form (equal mixture of two enantiomers R and S) in the international market. [0003] Clinical studies have shown that the pharmacological activity of ibuprofen is mainly produced by (S)-ibuprofen, and the drug activity of (S)-ibuprofen is 160 times that of (R)-ibuprofen; Profen not only has low activity, but also has toxic side effects. Since (S)-ibuprofen is a single enantiomer with pharmacokinetic activity, the use of (S)-ibuprofen at a dose lower than that of racemic ibuprofen can produce the same or even stronger pharmacological effects, even Less t...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C57/30
CPCC07B2200/07C07C51/42C07C57/30
Inventor 杨泓刘丽华窦春水刘增花朱伟伟
Owner 潍坊新益制药技术有限公司
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