Unlock instant, AI-driven research and patent intelligence for your innovation.

Diacerein crystal I and preparation method and application thereof

A kind of technology of diacerein and crystal form, applied in the field of diacerein crystal I and preparation thereof, can solve problems such as low absorption, low solubility of diacerein, low bioavailability, etc., achieve simple process, easy industrial Operation, good solubility

Active Publication Date: 2019-01-04
江苏德健医疗科技有限公司
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, due to the low solubility of diacerein, its in vivo behavior after oral administration will be limited, such as problems such as low absorption and / or low bioavailability

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Diacerein crystal I and preparation method and application thereof
  • Diacerein crystal I and preparation method and application thereof
  • Diacerein crystal I and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add diacerein (Hu Mengqi et al., A new method for the synthesis of diacerein, China Journal of Pharmaceutical Industry, 2017, 48 (9): 1270-1273) 1g, N, N-dimethyl Acetamide 6ml, heated at 70°C for 15min with stirring. Remove the heat, cool the feed solution to 250°C within 10 minutes in an ice-water bath at 0°C, keep it warm for 3 hours to crystallize; then filter with suction, rinse the filter cake with absolute ethanol, and dry under reduced pressure at 80°C to obtain diacerein crystals I 0.98g, yield 98%, purity 99.5%.

[0035] The 2θ of the X-ray powder diffraction pattern of the diacerein crystal I obtained above has characteristic absorption peaks at 6.5°, 11.0°, 13.5°, 21.1°, 23.4°, and 28.2°, and the error range of the 2θ value is ±0.2 °, X-ray powder diffraction pattern see figure 1 .

[0036] The diacerein crystal I obtained above has an endothermic peak at 249.2°C and a maximum endothermic peak at 252.5°C using DSC characterization. The crystal has a relat...

Embodiment 2

[0038] Add diacerein (Hu Mengqi et al., A new method for the synthesis of diacerein, China Journal of Pharmaceutical Industry, 2017, 48 (9): 1270-1273) 1g, N, N-dimethyl Acetamide 10ml, stirred and heated at 90°C for 15min. The heating was removed, and the feed solution was cooled to 25°C in an ice-water bath at 0°C within 10 minutes, and left to stand for crystallization for 1h. Suction filtration, rinse the filter cake with absolute ethanol, and dry under reduced pressure at 80°C to obtain 0.97 g of Diacerein Form I, with a yield of 97% and a purity of 99.5%.

[0039]The 2θ of the X-ray powder diffraction pattern of the diacerein crystal I obtained above has characteristic absorption peaks at 6.5°, 11.0°, 13.5°, 21.1°, 23.4°, and 28.2°, and the error range of the 2θ value is ±0.2 °, X-ray powder diffraction pattern see image 3 .

[0040] Referring to the method recorded in the article "Diacerein intervenes in the expression of connective tissue growth factor in cultured ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses diacerein crystal I and a preparation method and application thereof. The method includes: heating a mixture of diacerein and N,N-dimethylacetamide at 70-90 DEG C, and filtering to obtain filtrate; subjecting the filtrate to quick cooling, crystallizing and extraction filtration to obtain a filter cake; drying the filter cake to obtain the diacerein crystal I. A novel diacerein crystal form is provided, and stability in crystal form, high solubility, simplicity in process, high reproducibility and easiness in industrial operation and amplification are realized.

Description

technical field [0001] The invention relates to a diacerein crystal I and a preparation method and application thereof, belonging to the technical field of medicinal chemistry. Background technique [0002] The chemical name of Diacerein is 4,5-diacetyl-9,10-dihydro-9,10-dioxo-2-anthracenecarboxylic acid, and its structural formula is as follows: [0003] [0004] Studies have shown that the drug is used to treat degenerative joint diseases (osteoarthritis and related diseases), and can significantly improve symptoms such as pain and joint dysfunction caused by osteoarthritis and related diseases. -6 weeks, the effect is obvious. If the drug is stopped after 3 months of continuous treatment, the curative effect can last for at least 1 month (follow-up effect). [0005] Organic drug crystals are mostly molecular crystals, and different crystal forms can be obtained due to different crystallization conditions. This phenomenon is called polymorphism. The phenomenon of poly...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/16C07C67/52A61K31/222A61P19/02
CPCA61P19/02C07B2200/13C07C69/16
Inventor 常峰乐小勇胡代强李卫杰陈新
Owner 江苏德健医疗科技有限公司