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Perampanel crystal form a and preparation method thereof

A technology of crystal form and material crystal, applied to the crystal form of perampanel and the field of preparation thereof, can solve problems such as toxicity and environmental pollution, and achieve the effects of improved solubility, low cost and high solubility

Active Publication Date: 2017-03-01
CRYSTAL PHARMATECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing these anhydrous crystals, organic solvents such as acetone, methyl ethyl ketone, dichloromethane, methyl tert-butyl ether, and 2-methyltetrahydrofuran are used, all of which have certain toxicity and will cause environmental pollution to varying degrees. Pollution

Method used

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  • Perampanel crystal form a and preparation method thereof
  • Perampanel crystal form a and preparation method thereof
  • Perampanel crystal form a and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] The preparation method of perampanel crystal form A:

[0053] Add 50.1 mg of perampanel powder into 2.0 mL of a mixed solvent of acetic acid and water at a volume ratio of 1:1 to obtain a clear solution. Suspend and stir the solution for 1 day at room temperature, separate the solid by centrifugation, and dry it in vacuum for 24 After 1 hour, the solid was collected to obtain Form A. Table 1 shows the X-ray powder diffraction data of Form A obtained in this example. After testing its XRPD pattern and figure 1 Consistent, its DSC plot is consistent with figure 2 Consistent, its TGA diagram is consistent with image 3 unanimous.

[0054] Table 1 X-ray powder diffraction data of Form A

[0055] 2theta d interval strength% 7.44 11.89 100.00 8.79 10.07 10.25 9.55 9.27 24.10 12.01 7.37 9.72 14.23 6.22 5.24 15.18 5.84 16.74 15.56 5.70 3.24 17.35 5.11 17.50 19.20 4.62 18.09 20.70 4.29 2.96 22.93...

Embodiment 2

[0057] The preparation method of perampanel crystal form A:

[0058] Dissolve 10.3 mg of perampanel powder in 0.7 mL of a mixed solvent of acetic acid and water at a volume ratio of 5:2 to obtain a clear solution, heat the solution to 50°C, then slowly cool down to 5°C, and solids precipitate out. After vacuum drying for 24 hours, the solid was collected to obtain Form A. Table 2 shows the X-ray powder diffraction data of Form A obtained in this example.

[0059] Table 2 X-ray powder diffraction data of crystal form A

[0060] 2theta d interval strength% 7.43 11.90 100.00

[0061] 8.78 10.07 16.11 9.54 9.27 30.15 12.00 7.38 9.62 14.23 6.22 5.86 15.18 5.84 20.60 17.33 5.12 15.66 19.19 4.62 15.89 20.84 4.26 2.05 22.91 3.88 6.45 24.29 3.66 1.86 34.31 2.61 1.65 35.14 2.55 1.79 38.20 2.36 1.68

Embodiment 3

[0063] The preparation method of perampanel crystal form A:

[0064] Add 10.0 mg of perampanel powder to 0.5 mL of acetic acid and water in a mixed solvent with a volume ratio of 1:1 to obtain a suspension solution. Suspend and stir the solution for 1 day at room temperature, separate the solid by centrifugation, and dry in vacuo After 12 hours, the solid was collected to obtain Form A. Table 3 shows the X-ray powder diffraction data of Form A obtained in this example.

[0065] Table 3 X-ray powder diffraction data of Form A

[0066] 2theta d interval strength% 7.46 11.85 100.00 8.82 10.03 17.28 9.57 9.24 39.80 12.03 7.35 11.21 14.29 6.20 6.83 15.21 5.82 24.87 15.58 5.69 4.06 17.36 5.11 22.06 19.21 4.62 20.94 20.71 4.29 2.71 20.98 4.23 4.44 22.93 3.88 8.29 33.05 2.71 1.71 34.30 2.61 2.38

[0067] 35.14 2.55 3.06 38.18 2.36 2.31 39.04 2.31 1.41

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Abstract

The invention relates to a perampanel new type crystal A and a preparation method thereof. The new type crystal A is characterized in that an X-ray powder diffraction pattern has characteristic peaks when the 2 theta value is 7.4 plus or minus 0.2 degrees, 9.6 plus or minus 0.2 degrees, 19.2 plus or minus 0.2 degrees, 17.4 plus or minus 0.2 degrees, 15.2 plus or minus 0.2 degrees, 8.8 plus or minus 0.2 degrees, 12.0 plus or minus 0.2degrees, 22.9 plus or minus 0.2 degrees and 14.2 plus or minus 0.2 degrees.

Description

technical field [0001] The invention relates to the field of chemistry and medicine, in particular to a crystal form of perampanel and a preparation method thereof. Background technique [0002] Perampanel (the compound represented by formula I) was developed by Eisai, Japan, and was approved by the FDA on December 22, 2012 for the adjuvant treatment of partial seizures in epilepsy patients aged 12 years and above. Perampanel is an alpha-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA) receptor antagonist that reduces neuronal hyperexcitability by inhibiting postsynaptic AMPA receptor glutamate activity . This is the first FDA-approved antiepileptic drug with this mechanism of action. Its structure is as follows: [0003] [0004] Polymorphism exists widely in pharmaceuticals. Different crystal forms of the same drug have significant differences in solubility, melting point, density, and stability, which affect the stability, uniformity, bioavailability, effi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/64A61K31/444A61P25/08
CPCC07D213/64
Inventor 陈敏华张炎锋高岳君贝永燕刘启月
Owner CRYSTAL PHARMATECH CO LTD
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