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Crystal, preparation method and use thereof

A technology of crystal form and physical crystal, which is applied in the field of crystal, preparation and application, can solve problems such as interference, and achieve the effect of reducing diabetic complications

Active Publication Date: 2016-06-15
王军
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, hemihydrate crystal form A (US2008 / 0146515A1 crystal form) is easily obtained in an aqueous solvent system, which interferes with the preparation of crystal forms B and C

Method used

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  • Crystal, preparation method and use thereof
  • Crystal, preparation method and use thereof
  • Crystal, preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh about 10mg of 1-(β-D-glucopyranosyl)-4-methyl-3-[5-(4-fluorophenyl)-2-thienylmethyl]benzene into a glass bottle, at room temperature Add 0.4mL of n-octanol to dissolve the sample until clear, then place the sample at 5°C overnight (12h), the solid precipitates out, put the suspension in a filter centrifuge tube, and centrifuge at 4000rpm for 3 minutes. The obtained solid is detected by XRPD according to the method specified in this patent, and octanol and 1-(β-D-glucopyranosyl)-4-methyl-3-[5-(4-fluorobenzene) are detected by 1H NMR. base)-2-thienylmethyl] benzene molar ratio. The XRPD results show that the obtained solid position is crystal form III, octanol and 1-(β-D-glucopyranosyl)-4-methyl-3-[5-(4-fluorophenyl)-2-thiophene The molar ratio of methyl]benzene is 0.5:1. X-ray powder diffraction in this patent, the operation and analysis steps are as follows:

[0038] In CuKα radiation (1.54A), X-ray powder diffraction patterns are collected on the Bruker D8Disc...

Embodiment 2

[0044] Weigh about 10mg of 1-(β-D-glucopyranosyl)-4-methyl-3-[5-(4-fluorophenyl)-2-thienylmethyl]benzene into a glass bottle, at room temperature Add 0.5mL of n-octanol to dissolve the sample until clear, then gradually add 3.05mL of n-heptane, crystallize and precipitate a solid, place the suspension in a filter centrifuge tube, and centrifuge at 4000rpm for 3 minutes to obtain a solid. The XRPD method described in was detected as crystal form III.

Embodiment 3

[0046] Weigh about 10mg of 1-(β-D-glucopyranosyl)-4-methyl-3-[5-(4-fluorophenyl)-2-thienylmethyl]benzene into a glass bottle, room temperature Add 0.5mL of n-octanol under the conditions to dissolve the sample to clear, take 3mL of anti-solvent into a 20mL glass bottle, put the 1.5mL glass bottle containing the n-octanol solution of the compound into a 20mL glass bottle, let the anti-solvent gas Diffused into the sample solution, the suspension was placed in a filter centrifuge tube, centrifuged at 4000 rpm for 3 minutes, and the obtained solid was detected by the XRPD method described in Example 1, which was crystal form III. Here, n-hexane, pentane, cyclohexane, toluene, n-heptane, etc. can also be used as the anti-solvent.

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Abstract

Disclosed are crystal forms III and IV of 1-(β-D-pyranoglucosyl)-4-methyl-3-[5-(4-fluorophenyl)-2-thienyl methyl] benzene, at least having characteristic peaks where the 2θ value is 6.61±0.2, 3.92±0.2 and 19.68±0.2, and 17.40±0.2, 15.35±0.2 and 14.91±0.2 respectively in an X-ray powder diffraction pattern, and a preparation method and medicinal use thereof. The crystal form III is an octanol compound and has more remarkable effect in diabetes treatment; the crystal form IV is a non-hydrate and has high purity; the drying process for preparing the non-hydrate is simple, and the non-hydrate has obvious advantages over hydrate in respect to preparation process.

Description

technical field [0001] The present invention relates to a novel crystal of 1-(β-D-glucopyranosyl)-4-methyl-3-[5-(4-fluorophenyl)-2-thienylmethyl]benzene and a preparation method thereof and uses. Background technique [0002] Diabetes mellitus is a group of endocrine-metabolic diseases with hyperglycemia as its common sign. Disorders of sugar, protein, fat and secondary water and electrolyte metabolism caused by absolute or relative insufficient secretion of insulin. It can involve chronic damage and dysfunction of various systems of the whole body, especially the eyes, kidneys, heart, blood vessels, and nerves, and even induce many fatal complications. With the aging of the world population, diabetes has become a common and frequently-occurring disease, and it is a disease that seriously endangers human health. Research data show that the number of diabetic patients worldwide has increased from 150 million in 2000 to 280 million, and it is estimated that nearly 500 milli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D409/10A61K31/381A61P3/10A61P9/10A61P25/28A61P13/12A61P17/02A61P5/50A61P3/06A61P3/04A61P9/12A61P19/06
CPCC07D409/10A61K31/381
Inventor 王军
Owner 王军
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