FG-4592 single crystal and preparation method thereof
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A technology of FG-4592 and single crystal, which is applied in the field of medicine and can solve problems such as the preparation method of FG-4592 single crystal.
Inactive Publication Date: 2016-12-07
JIANGSU DEYUAN PHARMA
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[0006] There is no report on the preparation method of FG-4592 single crystal
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Embodiment 1
[0025] Example 1, a FG-4592 single crystal, its single crystal X-ray diffraction pattern has the following characteristics: the crystal belongs to the triclinic system, and the space group is P , the unit cell parameters are a=8.5830(17), b=9.2790(19), c=11.359(2)Å; α=99.16(3)°β=108.36(3)° γ=102.16(3)°, crystal Cell volume 814.2 (3) Å 3 , the number of molecules in the unit cell Z=2. Its X-ray diffraction pattern has the following characteristics: diffraction angle 2θ, interplanar distance d and relative intensity %, 2θ error is 0.2.
[0026] The preparation method of the FG-4592 single crystal is as follows: FG-4592 is dissolved in an organic solvent, the weight-to-volume ratio of the FG-4592 to the organic solvent is 1g:1ml; the dissolution method is ultrasonic dissolution, and the organic solvent is acetonitrile , anhydrous ethanol, acetone; naturally cool to room temperature after dissolving, add or not add solvent, seal, stand still, precipitate crystals, and filter to...
Embodiment 2
[0027] Example 2, a FG-4592 single crystal described in Example 1, its preparation method is as follows: FG-4592 is dissolved in an organic solvent, and the weight-to-volume ratio of the FG-4592 to the organic solvent is 1g:10ml; The dissolution method is ultrasonic dissolution, and the organic solvent is a combination of any two of acetonitrile, absolute ethanol, and acetone; after dissolution, it is naturally cooled to room temperature, with or without adding a dissolution agent, sealed, left standing, and crystals are precipitated, filtered Instantly.
Embodiment 3
[0028] Example 3, a FG-4592 single crystal described in Example 1, its preparation method is as follows: FG-4592 is dissolved in an organic solvent, and the weight-to-volume ratio of the FG-4592 to the organic solvent is 1g:40ml; The dissolution method is heating and dissolving at 30°C, and the organic solvent is a combination of three of acetonitrile, absolute ethanol, and acetone; after dissolving, naturally cool to room temperature, add or not add a dissolving agent, seal, stand still, and precipitate Crystals can be obtained by filtration.
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Abstract
The invention discloses an FG-4592 single crystal. The single crystal X-ray diffraction pattern of the FG-4592 single crystal is characterized in that the crystal belongs to a triclinic system, the space group is P (please see the formula in the specification), the cell parameter a is equal to 8.5830 (17), the cell parameter b is equal to 9.2790 (19), and the cell parameter c is equal to 11.359 (2) (please see the formula in the specification); alpha is equal to 99.16 (3) degrees, beta is equal to 108.36 (3) degrees, gamma is equal to 102.16 (3) degrees, the cell size is 814.2 (3)-<3> (please see the formula in the specification), and the number Z of molecules in a cell is equal to 2. The invention further discloses a method for preparing the FG-4592 single crystal. A simple solvent and a sample are matched to obtain the single crystal of FG-4592 fast, and the absolute configuration of the compound is obtained through a single crystal XRD. The crystal form of the sample can be determined through single crystal X-ray powder diffraction pattern simulation. The single crystal of FG-4592 is prepared, the absolute configuration and crystal form of the molecules can be obtained, the combination mode of the molecules and target protein (PHD) can be simulated through a molecular docking means, and the medicine effect achieving action mechanism of the single crystal is deeply known.
Description
technical field [0001] The invention relates to a single crystal of FG-4592 and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Anemia is the most common complication of chronic kidney disease (CKD) and tumors, and it is also an important risk factor leading to increased morbidity and mortality of CKD and cardiovascular complications. Anemia not only induces cardiovascular disease complications, but also is an important risk factor affecting hospitalization rate and mortality, and significantly affects the quality of life of patients. In China, studies have shown that the incidence of anemia increases with the decrease of renal function (increased number of CKD stages). [0003] Patients with renal anemia and tumor anemia have low levels of EPO. During treatment, EPO or EPO analogues are often injected to increase the level of EPO in the body, thereby helping patients increase the number of red blood cells. [0004]...
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