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Diacerein crystal and preparation method thereof

A diacerein and crystal technology, applied in the field of diacerein crystals, can solve the problems of unsatisfactory purification effect, low yield, cumbersome purification process, etc.

Active Publication Date: 2015-07-15
BEIJING WINSUNNY PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned purification process is cumbersome to operate, difficult to realize industrialization, low yield, and unsatisfactory purification effect

Method used

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  • Diacerein crystal and preparation method thereof
  • Diacerein crystal and preparation method thereof
  • Diacerein crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Mix 25ml of dimethylformamide and 80ml of acetone to obtain a mixed solvent, weigh 0.5g of diacerein and add it to the mixed solvent, heat and stir in a water bath at 65°C to dissolve, filter to remove insoluble matter, stand at 25°C for 6 hours, and a yellow color is precipitated The crystalline powder was suction filtered and dried to obtain 0.52 g of diacerein crystals. The resulting crystals have X-ray powder diffraction pattern data as shown below:

[0051]

Embodiment 2

[0053] Mix 37ml of dimethylformamide and 90ml of dichloromethane to obtain a mixed solvent, weigh 0.5g of diacerein and add it to the mixed solvent, heat and stir in a water bath at 50°C to dissolve, filter to remove insoluble matter, and stand at 30°C for 6.5 hours. A yellow crystalline powder was precipitated, filtered with suction, and dried to obtain 0.515 g of diacerein crystals. The X-ray powder diffraction spectrum data of the obtained crystal are the same as in Example 1.

Embodiment 3

[0055] Mix 30ml of dimethylformamide and 90ml of methanol to obtain a mixed solvent, weigh 1.0g of diacerein and add it to the mixed solvent, heat and stir in a water bath at 65°C to dissolve, filter to remove insoluble matter, and stand at 10°C for 8 hours, and a yellow color is precipitated The crystalline powder was suction filtered and dried to obtain 1.025 g of diacerein crystals. The X-ray powder diffraction spectrum data of the obtained crystal are the same as in Example 1.

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Abstract

The invention provides a method capable of efficiently obtaining high-purity diacerein, wherein the high-purity compound can be obtained by washing a diacerein solvate; at the same time, a crystalline morphology of the diacerein solvate and a preparation method for the crystalline morphology are provided.

Description

technical field [0001] The invention relates to a diacerein crystal for treating degenerative bone and joint diseases, a preparation method of the crystal and a method for purifying the diacerein. Background technique [0002] Diacerein is a new interleukin (IL-1) inhibitor. Clinical studies have shown that diacerein can significantly improve the joint function of patients with osteoarthritis, delay the course of the disease, relieve pain, and improve the quality of life of patients. With stronger follow-up effect and better safety than NSAIDs, it is an effective drug for treating osteoarthritis. The chemical name is 4,5-diacetyl-9,10-dihydro-9,10-dioxo-2-anthracenecarboxylic acid. Its specific structural formula is: [0003] [0004] The synthesis of diacerein has been reported in many literatures. Most of these literatures use aloin as the starting material. After its hydroxyl group is acetylated, it is oxidized with chromic anhydride in acetic acid to obtain diacere...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/16C07C67/52C07C67/48A61K31/222A61P19/02A61P29/00
CPCC07B2200/13C07C67/48C07C67/52C07C69/16
Inventor 周浩辉林国良张保国王圣涛
Owner BEIJING WINSUNNY PHARMA CO LTD
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