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Methods for preparing voriconazole crystal form I

A technology for voriconazole crystal and voriconazole, which is applied in the field of preparing voriconazole crystal form I, can solve the problems of cumbersome methods, unfavorable industrial production, poor reproducibility and the like, and achieves the effects of avoiding uncontrollability and increasing controllability and stability.

Active Publication Date: 2015-08-19
INST OF MATERIA MEDICA CHINESE ACAD OF MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method involves repeated extraction, washing, stirring, filtering, solvent removal and other steps, the method is cumbersome and has poor reproducibility, which is not conducive to industrial production

Method used

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  • Methods for preparing voriconazole crystal form I
  • Methods for preparing voriconazole crystal form I
  • Methods for preparing voriconazole crystal form I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] A sample of 1g of voriconazole was completely dissolved in 40mL of n-propanol under heating at 60°C, filtered, and the filtrate was placed at room temperature for 3 days to crystallize. The solution was removed by filtration to obtain a solid sample, which was vacuum dried at 40°C for 12 hours to obtain 0.91g voriconazole crystal form sample, melting point 129.5~130.5℃, yield 91%, powder X-ray diffraction analysis of the obtained sample, the diffraction pattern is consistent with figure 1 Consistent, indicating that the obtained sample is a voriconazole crystal type I solid substance with high crystal purity.

Embodiment 2

[0068] A sample of 1g voriconazole was completely dissolved in 15mL of dichloromethane under heating at 50°C, filtered, and the filtrate was placed at -10°C for 2 days to crystallize. The solution was removed by filtration to obtain a solid sample, which was vacuum dried at 40°C for 12 hours , Obtain 0.92g voriconazole crystal form sample, the melting point is 129.5~130.5℃, the yield is 92%, the obtained sample is subjected to powder X-ray diffraction analysis, the diffraction pattern is consistent with figure 1 Consistent, indicating that the obtained sample is a voriconazole crystal type I solid substance with high crystal purity.

Embodiment 3

[0070] A 1g sample of voriconazole was completely dissolved in 15mL of acetone under heating at 50°C, filtered, and the filtrate was placed at -5°C for 2 days to crystallize. The solution was removed by filtration to obtain a solid sample, which was vacuum dried at 40°C for 12 hours to obtain 0.93g voriconazole crystal form sample, melting point 129.5~130.5℃, yield 93%, powder X-ray diffraction analysis of the obtained sample, its diffraction pattern is consistent with figure 1 Consistent, indicating that the obtained sample is a voriconazole crystal type I solid substance with high crystal purity.

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Abstract

The present invention relates to a plurality of new methods for preparing a voriconazole crystal form I, wherein the methods comprise a different solvent re-crystallization method, a fast rotary evaporation method, a melting cooling method and the like. According to the present invention, the obtained voriconazole crystal type I is subjected to powder X-ray diffraction analysis, DSC analysis and infrared spectroscopy analysis, and the results show that the prepared crystal form I belongs to the high purity crystal form; and the voriconazole crystal form I can be rapidly prepared by using the method of the present invention, and the method has characteristics of high crystal form purity, less impurity, simple operation, easy industrial production, and great practical application value.

Description

Technical field [0001] The present invention relates to the discovery of multiple preparation methods of Voriconazole crystal form I. Background technique [0002] Voriconazole is a triazole compound with a chemical name of (2R,3S)-2-(2,4-difluorophenyl)-3-(5-fluoropyrimidin-4-yl)-1-(1H- 1,2,4-triazol-1-yl)-2-butanol, its structural formula is shown below, [0003] [0004] Voriconazole is a second-generation broad-spectrum triazole antifungal developed by Pfizer based on the structure of fluconazole. It is mainly used to treat invasive aspergillosis and severe invasion caused by fluconazole-resistant Candida Sexual infection, with good pharmacokinetic characteristics. The drug underwent phase III clinical trials in 1996 and was officially approved by the US FDA for marketing in June 2002. [0005] International patent WO2006065726A2 discloses the crystal form A and crystal B of voriconazole, and at the same time, some pharmaceutical excipients are used to prepare the amorphous fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D403/06
CPCC07B2200/13C07D403/06
Inventor 吕扬杜冠华张宝喜周政政杨世颖
Owner INST OF MATERIA MEDICA CHINESE ACAD OF MEDICAL SCI