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Preparation method of arbidol methanesulfonate crystal

A technology of Arbidol and methanesulfonic acid, which is applied in the field of preparation of drug crystal forms, can solve problems such as difficult storage, easy water absorption, instability, etc., and achieve the effect of fewer reagents, good stability, and fewer steps

Active Publication Date: 2013-09-11
HUBEI LIYI PHARM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Arbidol mesylate amorphous powder, easy to absorb water, unstable, difficult to store

Method used

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  • Preparation method of arbidol methanesulfonate crystal
  • Preparation method of arbidol methanesulfonate crystal
  • Preparation method of arbidol methanesulfonate crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of Arbidol mesylate crystal form, the steps are as follows:

[0031] Dissolve 5.7g of Arbidol in 50mL of acetone, heat to 50°C, then add 1.49g of methanesulfonic acid, stir the reaction for 1h, cool to room temperature, stir at 500rpm overnight (12h), filter with suction, and wash the solid with isopropanol After washing twice and drying in vacuum, 5.5 g of Arbidol mesylate crystals was obtained, with a yield of 80.2%. The product was detected by HPLC with a purity of 99.6% and a melting point of 167.5-168.5°C.

Embodiment 2

[0033] A preparation method of Arbidol mesylate crystal form, the steps are as follows:

[0034] Dissolve 5.7g of Arbidol in 40mL of absolute ethanol, heat to 45°C, then add 1.49g of methanesulfonic acid, stir the reaction for 0.5h, cool to room temperature, stir at 300rpm overnight (14h), filter with suction, and use the solid After washing with isopropanol for 3 times and drying in vacuo, 5.1 g of Arbidol mesylate crystals was obtained with a yield of 74.4%. The purity of the product was 99.6% and the melting point was 167.5-168.5° C. as detected by HPLC.

Embodiment 3

[0036] A preparation method of Arbidol mesylate crystal form, the steps are as follows:

[0037] Dissolve 5.7g of Arbidol in 40mL of dichloromethane, heat to 55°C, then add 1.49g of methanesulfonic acid, stir the reaction for 1.5h, cool to room temperature, stir at 700rpm overnight (10h), filter with suction, and use the solid After washing twice with isopropanol and drying in vacuo, 5.8 g of Arbidol mesylate crystals was obtained with a yield of 84.6%. The purity of the product was 99.7% and the melting point was 167.5-168.5° C. as detected by HPLC.

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Abstract

The invention discloses a preparation method of an arbidol methanesulfonate crystal, which comprises the following steps: dissolving active pharmaceutical ingredient arbidol in an organic solvent, heating to 45-55 DEG C, adding methanesulfonic acid, stirring to react for 0.5-1.5 hours, cooling, continuing stirring for 10-14 hours until the crystal precipitates, filtering to collect the precipitate crystal, washing the crystal with isopropanol 1-3 times, and carrying out vacuum drying to obtain the low-hygroscopicity arbidol methanesulfonate crystal which can satisfy the demand for pharmaceutical preparation stability. The purity of the arbidol methanesulfonate crystal is higher than 99.5%.

Description

technical field [0001] The invention relates to the technical field of preparation of pharmaceutical crystal forms, in particular to a method for preparing a pharmaceutically acceptable crystal form of Arbidol mesylate, a drug for treating and preventing influenza virus. Background technique [0002] At present, the antiviral chemical drugs used clinically at home and abroad mainly include arbidol, ribavirin, amantadine, rimantadine, oseltamivir, and zanamivir. Among them, ribavirin is active against influenza A and B viruses when used in large doses, but it has the teratogenic and mutagenic toxicity of nucleoside drugs, which can cause anemia and immunosuppression. Amantadine and rimantadine are only effective against influenza A, and are prone to drug resistance. Such drugs can also cause toxic reactions in the central nervous system, thereby reducing the clinical use value. The neuraminidase inhibitors oseltamivir and zanamivir are effective but expensive. [0003] Arb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/42
Inventor 陈龙舒志元李霞刘胜文方征远李旻
Owner HUBEI LIYI PHARM TECH CO LTD