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Crystal form of deuterium tryptophan hydroxylase inhibitor

A crystal form and crystallization technology, which is applied in the field of crystal form and preparation of deuterated tryptophan hydroxylase inhibitors, can solve the problem of unstable physical and chemical properties of amorphous form, difficult handling and preparation of amorphous drug substances , unreliable solubility and other issues

Inactive Publication Date: 2019-01-11
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

[0003] Amorphous drug substances are known to not be a good solution to the above problems
For example, amorphous drug substances are often difficult to handle and formulate, offer unreliable solubility, and are often found to be physically and chemically unstable in the amorphous form

Method used

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  • Crystal form of deuterium tryptophan hydroxylase inhibitor
  • Crystal form of deuterium tryptophan hydroxylase inhibitor
  • Crystal form of deuterium tryptophan hydroxylase inhibitor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the preparation of crystal form A

[0026]

[0027] Add 2g of the compound of formula (I) to 25g of N-methylpyrrolidone, start stirring, stir for 2h under heating and reflux, stop heating, stir and cool to room temperature, and continue stirring for 1h. The resulting suspension was filtered with suction, the filter cake was washed with a small amount of ether, the filter cake was collected, and dried under vacuum at 45° C. to obtain 1.6 g of crystals of the compound of formula I in Form A. DSC test melting point: 185°C.

[0028] Tested by X-ray powder diffraction, using Cu-Kα radiation, with the following characteristic peaks expressed in angle 2θ: 7.36°±0.2°, 9.52°±0.2°, 10.66°±0.2°, 14.54°±0.2°, 15.29° ±0.2°, 17.28°±0.2°, 18.15°±0.2°, 19.27°±0.2°, 20.96°±0.2°, 25.34°±0.2°, 30.62°±0.2°, 31.38°±0.2°.

Embodiment 2

[0029] Embodiment 2: content stability test

[0030] The compound crystal form A crystal of formula I has been studied on the content stability; Humidity 75% ± 5%) and long-term test (temperature 25 ℃ ± 2 ℃, relative humidity 60% ± 10%) carry out high performance liquid chromatography detection content to the sample, test result is as follows:

[0031]

Embodiment 3

[0032] Embodiment 3: crystal formation stability test

[0033] Stability studies have been carried out on the compound crystal form A of formula I;: [high temperature (60°C), high humidity (90% ± 5%), light (4500lx)], accelerated test (temperature 40°C ± 2°C, relative humidity 75%±5%) and long-term test (temperature 25℃±2℃, relative humidity 60%±10%) and X-ray powder diffraction test on the sample after grinding and tableting. The test results are as follows:

[0034]

[0035]

[0036] The test results show that the XRPD main 2θ angles of this product after grinding and tableting do not change significantly, indicating that the crystal form of this product has good stability during the preparation process. In addition, after 6 months of accelerated testing and 12 months of long-term sample retention, the crystal form of this product has not changed significantly, indicating that the crystal form of this product is stable during storage and meets the needs of medicinal us...

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Abstract

The invention relates to a crystal form of a deuterium tryptophan hydroxylase inhibitor and a preparation method thereof and in particular relates to a crystal form of a compound of formula (I), and apreparation method of the crystal form of the compound. Stability test and solubility test results show that the crystal form of the compound of formula (I) provided by the invention meets the medicinal demands. The structural formula is as shown in the specification.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a crystal form of a deuterated tryptophan hydroxylase inhibitor 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 formulate, pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D403/12A61P1/12A61P35/00A61K31/506
CPCA61P1/12A61P35/00C07B2200/05C07B2200/13C07D403/12
Inventor 邓泽平陈芳军王岳奇唐立明李斌
Owner 湖南华腾制药有限公司
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