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Racemic dihydromyricetin monohydrate crystal

A technology of dihydromyricetin and monohydrate, which is applied in the field of medicine and can solve problems such as inability to reveal the crystal structure

Inactive Publication Date: 2016-10-12
TONGJI HOSPITAL ATTACHED TO TONGJI MEDICAL COLLEGE HUAZHONG SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the presence of more hydrogen bonds in the dihydromyricetin molecule, which can form intramolecular and intermolecular hydrogen bonds, and may also contain crystal water, only from the compound at 3300cm -1 There is a broad peak at , which cannot indicate its crystal structure

Method used

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  • Racemic dihydromyricetin monohydrate crystal
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  • Racemic dihydromyricetin monohydrate crystal

Examples

Experimental program
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Embodiment 1

[0073] The preparation of embodiment 1 D-dihydromyricetin dihydrate

[0074] Take about 200mg of D-dihydromyricetin raw material, which can be anhydrous or monohydrate, dissolve it in 2ml of 90-100°C aqueous solution, filter with heat preservation, remove the filter residue, and cool the solution naturally to room temperature to precipitate crystals. Get D-dihydromyricetin dihydrate.

Embodiment 2

[0075] The preparation of embodiment 2 D-dihydromyricetin anhydrate

[0076] Take about 200 mg of D-dihydromyricetin raw material, which can be dihydrate or monohydrate, and place it at a temperature of 160 ° C for 1 hour to obtain dihydromyricetin anhydrate.

Embodiment 3

[0077] The preparation of embodiment 3 D-dihydromyricetin monohydrate

[0078] Take about 200 mg of D-dihydromyricetin raw material, which can be dihydrate or anhydrous, dissolve in high-concentration ethanol solution, volatilize slowly until crystallization, and obtain D-dihydromyricetin monohydrate.

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Abstract

The invention discloses a racemic dihydromyricetin monohydrate crystal. A dihydromyricetin stereo-configuration is characterized by a specific rotation method and a high performance liquid phase chiral splitting method. With use of solid analysis techniques including single crystal X-ray diffraction, powder X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Karl Fischer titration and Fourier transform attenuated total reflection infrared spectrometry (FT-ATR), a dihydromyricetin crystal form is characterized; the dihydromyricetin is subjected to polymorphism screening and has important significance to raw material drug technology development and development and quality control of solid preparations, semi-solids, suspensions and other preparation forms.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a racemic crystal of dihydromyricetin monohydrate. Its branch case is in the Chinese invention patent "Dihydromyricetin five different crystal forms" with application number 2014107158285. Background technique [0002] Dihydromyricelin, also known as Ampelopsin, was first isolated by Kotake and Kubota in 1940 from the leaves of Ampelopsis meliaefolia, a dihydroflavone Alcohol flavonoid compound, the chemical structure is 3,5,7,3',4',5'-hexahydroxy-2,3-dihydroflavonol. Dihydromyricetin is widely found in the genus Vitaceae of the Vitaceae family, and also in the plants of Myriceaceae, Rhododendronaceae, Garciniaceae, Euphorbiaceae, Olives, Fabaceae, Sapotaceae and Salicaceae. [0003] Dihydromyricetin is white or light yellow needle-like crystal, poorly water-soluble (0.2mg / ml, 25℃), easily soluble in hot water, ethanol, methanol, acetone and DMSO. The chemical stability of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/32C07D311/40
CPCC07D311/32C07B2200/13C07D311/40
Inventor 施春阳方建国王文清熊微陈婧刘旭王晨光侯小龙
Owner TONGJI HOSPITAL ATTACHED TO TONGJI MEDICAL COLLEGE HUAZHONG SCI TECH
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