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New crystal form of nifuratel and preparation method and application thereof

A technology of nifuratel and crystal form, applied in the field of chemical pharmacy, can solve the problems of increased nifuratel, low yield and the like, and achieves the effects of short operation time, high yield and good solubility

Inactive Publication Date: 2019-04-19
BEIJING JINCHENG TAIER PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] There are a large number of documents and patents to study the technology of nifuratel at present, and there is no report on its crystal form research. The refining method of nifuratel in the prior art is mainly glacial acetic acid refining, because nifuratel Er is a Schiff base compound, which is easily degraded under acidic and high temperature conditions, and has a large solubility in glacial acetic acid, with a yield of about 80%.
Patent CN103664923B selects N, N-dimethylformamide and dioxane as the crystallization solvent through optimization, and the stability of nifuratel is increased, but the yield is still low, between 79% and 82%.

Method used

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  • New crystal form of nifuratel and preparation method and application thereof
  • New crystal form of nifuratel and preparation method and application thereof
  • New crystal form of nifuratel and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Under dark conditions, add 100.0g nifuratel, 300ml DMF to a 1000ml reaction flask, heat to 50℃, stir until the solid is clear, add 1.0g activated carbon, decolorize for 1h, filter out the activated carbon, and transfer the filtrate to another In a 2000ml reaction flask, heat up to 50°C, add 900ml purified water dropwise, after the addition is complete, drop the temperature to 25°C, filter with suction, rinse the filter cake with purified water and ethanol successively, drain off, and blow the solid at 80°C After drying for 10 hours, a yellow solid nifuratel crystal form B, 96.5 g, was obtained, the yield was 96.5%, and the HPLC purity was 99.9%. The X-powder diffraction pattern of nifuratel crystal form B prepared in Example 1 is shown in figure 1 ; The DSC spectrum of nifuratel crystal form B prepared in Example 1 is shown in figure 2 .

Embodiment 2

[0040] Under dark conditions, add 100.0g nifuratel, 200ml DMF to a 1000ml reaction flask, heat to 50℃, stir until the solid is clear, add 1.0g activated carbon, decolorize for 1h, filter out the activated carbon, and transfer the filtrate to another In a 2000ml reaction flask, heat up to 60℃, and add 600ml purified water dropwise. After the addition is complete, drop the temperature to 30°C, suction and filter, the filter cake is rinsed with purified water and ethanol in turn, drained, and the solid is blown at 70°C. After drying for 12 hours, a yellow solid nifuratel crystal form B was obtained, 95.3 g, with a yield of 95.3% and an HPLC purity of 99.9%.

Embodiment 3

[0042] Under dark conditions, add 100.0g nifuratel, 500ml DMF to a 1000ml reaction flask, heat to 50℃, stir until the solid is clear, add 1.0g activated carbon, decolorize for 1h, filter out the activated carbon, and transfer the filtrate to another In a 2000ml reaction flask, the temperature is raised to 50°C, and 1000ml of purified water is added dropwise. After the addition is complete, the temperature is lowered to 25°C. The filter cake is rinsed with purified water and ethanol in turn, drained, and the solid is blown at 90°C. After drying for 8 hours, a yellow solid crystal form B of nifuratel was obtained, 95.1 g, with a yield of 95.1% and an HPLC purity of 99.8%.

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Abstract

The invention belongs to the technical field of chemical pharmacy, and particularly relates to a new crystal form of nifuratel and a preparation method and application thereof. The peak values of 2 theta in the X-ray powder diffraction pattern are 6.00 + / - 0.2,7.77 + / - 0.2,11.98 + / - 0.2,13.86 + / - 0.2,15.58 + / - 0.2,17.50 + / - 0.2,19.89 + / - 0.2,21.73 + / - 0.2 degrees. The new crystal form is stable incrystal form, and simultaneously has good high-humidity stability, solubility and good dissolution property; the invention also provides a preparation method of the new nifuratel crystal form, whichis low in carbon and environment-friendly, and the used solvent is cheap and easy to obtain, low in toxicity, good in process route stability, strong in operability, high in product purity and high inyield, which is very suitable for long-time storage, and is suitable for industrial production; the invention also provides an application of the new crystal form of nifuratel, so that the nifuratelsolid preparation with good pharmaceutical characteristics can be prepared.

Description

Technical field [0001] The invention belongs to the technical field of chemical pharmacy, and specifically relates to a new crystal form of nifuratel and a preparation method and application thereof. Background technique [0002] Nifuratel, chemical name: 5-[(methylthio)methyl]-3-{[(5-nitro-2-furan)methylene]amino}-2-oxazolidinone, English name : Nifutatel is a drug mainly used for gynecological infections developed and produced by Italy's Puli Chemical Company. This drug is a broad-spectrum antibiotic, especially for the common pathogens of gynecological infections such as Gram-positive and negative bacteria, drops Insects, molds, chlamydia and mycoplasma have a strong killing effect, and have a good effect on the treatment of common gynecological vaginal infections caused by trichomoniasis, candida albicans, bacteria, etc. Now it is marketed in my country and many other countries in dosage forms such as tablets, capsules, and suppositories. [0003] The chemical structure of ni...

Claims

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Application Information

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IPC IPC(8): C07D413/12A61K31/422A61P31/04A61P15/00A61P31/10A61P33/02
CPCA61P15/00A61P31/04A61P31/10A61P33/02C07B2200/13C07D413/12
Inventor 伊茂聪张新余王晓光王丽霞
Owner BEIJING JINCHENG TAIER PHARMA CO LTD
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