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Crystal form of trifluoromethyl replaced imidazole diketone type derivative

A technology of crystal form and dimethylformamide, which is applied in the field of crystal form and preparation of imidazole diketone derivatives, and can solve problems such as no crystal form

Inactive Publication Date: 2018-12-28
湖南华腾制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The Chinese patent application number is 201810658773.7, which has applied for the corresponding protection of the compound of formula (I), its preparation method and use, but there has been no relevant report on the crystal form so far

Method used

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  • Crystal form of trifluoromethyl replaced imidazole diketone type derivative
  • Crystal form of trifluoromethyl replaced imidazole diketone type derivative
  • Crystal form of trifluoromethyl replaced imidazole diketone type derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Compound 1:

[0034] Preparation of Form A-1:

[0035] Compound 1 (100 g) was added to N,N-dimethylformamide (1.5 L), heated to reflux to dissolve, then refluxed for 2.5 h, then cooled and stirred for 14 h to crystallize. After filtering, the filter cake was washed with ether, and the resulting solid was dried under reduced pressure at 60°C to constant weight. The target product (96.4 g, off-white solid) was obtained with a yield of 96.4%.

[0036] Stability experiment:

[0037] The stability study was carried out on the compound 1 crystal form A-1 crystal: the samples were placed for 0 months and 6 The X-ray powder diffraction test was carried out in each month, and the test results are as follows:

[0038] Instrument model: D / Max-RA Japan Rigaku X-ray powder diffractometer

[0039] Rays: monochromatic Cu-Kα rays

[0040] Scanning mode: θ / 2θ, scanning range: 3-45°

[0041] Temperature range: 294K Voltage: 40KV

[0042] The comparison of X-ray diffraction data i...

Embodiment 2

[0049] Compound 2:

[0050] Preparation of Form A-2:

[0051] Compound 2 (100g) was added into N,N-dimethylformamide (1.5L), heated to reflux to dissolve, then refluxed for 2h, then cooled and stirred for 10h to crystallize. After filtering, the filter cake was washed with ether, and the resulting solid was dried under reduced pressure at 65°C to constant weight. The target product (96.1 g, off-white solid) was obtained with a yield of 96.1%.

[0052] Example 2

[0053] Stability experiment:

[0054] The stability study was carried out on the compound 2 crystal form A-2 crystal: under the conditions of accelerated test (light (4500lx), temperature 40 ℃ ± 2 ℃, relative humidity 75% ± 5%), the sample was placed for 0 months and 6 months The X-ray powder diffraction test was carried out in each month, and the test results are as follows:

[0055] Instrument model: D / Max-RA Japan Rigaku X-ray powder diffractometer

[0056] Rays: monochromatic Cu-Kα rays

[0057]Scanning mod...

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PUM

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Abstract

The invention relates to a crystal form of a trifluoromethyl replaced imidazole diketone type derivative and a preparation method of the trifluoromethyl replaced imidazole diketone type derivative, inparticular to a crystal form of a compound as shown in the formula (I) and a preparation method of the compound. Stability test and dissolvability test results show that the crystal form of the compound as shown in the formula (I) provided by the invention meets medical requirement. (As shown in the description).

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a crystal form of trifluoromethyl-substituted imidazoledione derivatives and a preparation method thereof. Background technique [0002] Chemical stability, solid state stability and "shelf life" of drug substances are particularly important factors in the manufacture of pharmaceuticals. It is important to identify forms of drugs that can be conveniently prepared, formulated and administered to patients. An ideal drug substance and compositions containing it can be effectively stored during the evaluation period without showing significant changes in the physicochemical properties of the active ingredient (such as chemical composition, density, hygroscopicity, solubility and dissolution rate, etc.). [0003] It is known that amorphous drug substances do not solve the above problems well. For example, amorphous drug substances are often difficult to handle and form...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D403/04
CPCC07B2200/13C07D403/04
Inventor 许慧陈芳军唐立明王岳奇
Owner 湖南华腾制药有限公司