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Benvitimod impurity as well as preparation method and application thereof

A technology of phenylene moder and impurity, which is applied in the field of drug synthesis to achieve the effect of strengthening control, ensuring safety and effectiveness, and improving quality

Pending Publication Date: 2021-06-25
广东中昊药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first condition for drug impurity research is to obtain impurity control samples. However, there are few reports on phenylene moder impurities and their preparation processes. Therefore, it is necessary to develop benzoyl moder-related impurities and their preparation methods for Quality control of raw materials and preparations

Method used

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  • Benvitimod impurity as well as preparation method and application thereof
  • Benvitimod impurity as well as preparation method and application thereof
  • Benvitimod impurity as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] As an embodiment of the preparation method of the phenylene Moder impurity described in the present invention, the preparation method of the Benzene Moder impurity described in this embodiment comprises the following steps:

[0039] (1) Take 1 kg of E-1,3-dimethoxy-2-isopropyl-5-(2-styryl)-benzene and 2.0 kg of pyridine hydrochloride, put them in a reaction vessel, heat and keep Stir the reaction at 200°C, monitor by HPLC, stop the reaction until the reaction of E-1,3-dimethoxy-2-isopropyl-5-(2-styryl)-benzene is complete;

[0040] (2) Take 13.0L of ethyl acetate, 9.0L of drinking water and 0.28L of hydrochloric acid, put them in the extraction container, stir, transfer the reaction solution in step (2) to the extraction container while it is hot, stir, let it stand, and discard the lower layer Water phase; add 8.5L drinking water and 0.14L hydrochloric acid, stir, let stand, discard the lower aqueous phase; add 4.0L drinking water, stir, let stand, discard the lower aq...

Embodiment 2

[0052] As an embodiment of the preparation method of the phenylene Moder impurity described in the present invention, the preparation method of the Benzene Moder impurity described in this embodiment comprises the following steps:

[0053] (1) Take E-1,3-dimethoxy-2-isopropyl-5-(2-styryl)-benzene Akg and pyridine hydrochloride 2.0Akg, place in a reaction vessel, heat, keep Stir the reaction at a temperature of 140°C, monitor by HPLC, until the reaction of E-1,3-dimethoxy-2-isopropyl-5-(2-styryl)-benzene is complete, and the reaction time is 20h to stop the reaction;

[0054] (2) Take 13.0AL tetrahydrofuran, 9.0AL drinking water and 0.28L sulfuric acid, put them in the extraction container, stir, transfer the reaction solution in step (2) to the extraction container while it is hot, stir, let it stand, and discard the lower layer water phase; add 8.5A L of drinking water and 0.14A L of sulfuric acid, stir, let stand, discard the lower water phase; add 4.0A L of drinking water, ...

Embodiment 3

[0059] As an embodiment of the preparation method of the phenylene Moder impurity described in the present invention, the preparation method of the Benzene Moder impurity described in this embodiment comprises the following steps:

[0060] (1) Take A kg of E-1,3-dimethoxy-2-isopropyl-5-(2-styryl)-benzene and 2.0 Akg of pyridine hydrochloride, place it in a reaction vessel, heat, Keep the temperature at 220°C, stir the reaction, monitor by HPLC, until the reaction of E-1,3-dimethoxy-2-isopropyl-5-(2-styryl)-benzene is complete, the reaction time is 2h, stop the reaction ;

[0061] (2) Take 13.0A L of methyl tert-butyl ether, 9.0A L of drinking water and 0.28L of acetic acid, put them in the extraction container, stir, transfer the reaction solution in step (2) to the extraction container while it is hot, stir, and let stand , discard the lower water phase; add 8.5AL drinking water and 0.14A L acetic acid, stir, let stand, discard the lower water phase; add 4.0A L drinking wate...

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Abstract

The invention discloses a benvitimod impurity as well as a preparation method and application thereof. The prepared benvitimod impurity is high in purity and can be used as an impurity reference substance in benvitimodbulk drug or preparation detection, accurate positioning of the impurity 6-methyl-5-[(E)-2-styryl]-2-isopropyl-1,3-benzenediol in production quality control of benvitimod is improved, control over the impurity is enhanced, and the quality of the benvitimod preparation is improved, so that the safety and the effectiveness of the benvitimod preparation in clinical use are ensured.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a benzophenone moder impurity and its preparation method and application. Background technique [0002] Benzenemod is a non-hormonal, low-toxic small molecule compound (mw=254) discovered and isolated from the metabolites of soil nematode symbiotic bacteria. It has unique lymphase inhibitory biological activity and can be used to treat various Major autoimmune diseases such as psoriasis, eczema, pyogenic colitis and various allergic diseases. The chemical name of phenylene moder is 5-[(E)-2-styryl]-2-isopropyl-1,3-benzenediol, and its structure is shown in formula I: [0003] [0004] One of the main factors affecting drug quality is drug impurities. Impurity research is an important part of drug research. Whether impurities can be reasonably and effectively controlled is directly related to the quality controllability and safety of drugs. Therefore, the control of st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/21C07C37/055C07C37/72C07C37/82G01N30/02G01N30/06G01N30/86
CPCC07C37/055C07C37/72C07C37/82C07C39/21G01N30/02G01N30/06G01N30/8675
Inventor 蒋荣林胡四进温雄学
Owner 广东中昊药业有限公司
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