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New crystal form of istradefylline and preparation method thereof

A crystal form and crystal technology, applied in the field of medicine, can solve problems such as many adverse reactions, poor tolerance, and reduced curative effect

Inactive Publication Date: 2016-08-24
南京瑞天医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although levodopa is the main drug for the treatment of Parkinson's disease, due to its poor tolerance and many adverse reactions, such as vomiting, involuntary movement dysfunction, and long-term use, the curative effect is reduced, and a new treatment method is urgently needed

Method used

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  • New crystal form of istradefylline and preparation method thereof
  • New crystal form of istradefylline and preparation method thereof
  • New crystal form of istradefylline and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1 Preparation of istradefylline crystal form IV

[0021] Weigh 1g of istradefylline into a 50ml single-necked bottle, then add 15ml of n-propanol, stir and heat to 100°C, continue stirring for 3h until reflux occurs, stop heating, cool to room temperature while stirring and crystallizing. The resulting suspension was suction-filtered, the filter cake was washed with 10 ml of n-propanol, and dried at 50°C to constant weight to obtain 0.89g of istradefylline Form IV, with a melting point of 192.8°C as determined by DSC.

Embodiment 2

[0022] Embodiment 2 Preparation of istradefylline crystal form IV

[0023] Weigh 1g of istradefylline into a 50ml single-necked bottle, then add 25ml of n-propanol, stir and heat to 110°C, continue stirring for 6h until reflux occurs, stop heating, cool to room temperature while stirring and crystallizing.

[0024] The obtained suspension was suction-filtered, the filter cake was washed with 10 ml of n-propanol, and dried at 50°C to constant weight to obtain 0.85 g of istradefylline Form IV, with a melting point of 192.9°C as determined by DSC.

Embodiment 3

[0025] Example 3 Stability study of istradefylline crystal form IV

[0026] Stability studies have been carried out on istradefylline crystal form IV: [high temperature (60°C), high humidity (90%±5%), light (45001X)], accelerated test (temperature 40±2°C, relative humidity 75% ±5%) and long-term test (temperature 25±2°C, relative humidity 60%±10%)] and carry out X-ray powder diffraction test on the sample after grinding and tableting.

[0027] Table 1 Results of determination of stability of crystal form IV

[0028]

[0029] Table 2 Crystal Form IV Influencing Factor Test Determination Results

[0030]

[0031]

[0032] Table 3 Form IV Stability Test Determination Results

[0033]

[0034] The test results show that: after grinding and tableting, the X-ray diffraction test shows that the crystal form data of this product has not changed significantly, indicating that this product has good stability during the preparation process. In the test of influencing facto...

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Abstract

The invention relates to a new crystal form of istradefylline and a preparation method thereof; the new crystal form IV has a powder X-ray diffraction pattern having main characteristic absorption peaks at diffraction angles (2theta) of 5.763 degrees, 6.958 degrees, 10.599 degrees, 10.999 degrees, 13.944 degrees, 15.647 degrees, 19.513 degrees, 21.004 degrees, 21.400 degrees, 24.426 degrees and 28.320 degrees. The invention also discloses the preparation method of the new crystal form IV which has simple preparation process and relatively good stability and conforms to medicinal requirements.

Description

technical field [0001] The invention belongs to the technical field of medicine, and specifically relates to (E)-8-[2-(3,4-dimethoxyphenyl)vinyl]-1,3-diethyl-3,7-dihydro - A new crystal form IV of 7-methyl-1H-purine-2,6-dione (Itradefylline) and a process for its preparation. Background technique [0002] Itradefylline (Istradefylline, KW6002), chemical name (E)-8-[2-(3,4-dimethoxyphenyl) vinyl]-1,3-diethyl-3,7-di Hydrogen-7-methyl-1H-purine-2,6-dione, formula C 20 h 24 N 4 o 4 , molecular weight 384.43, CAS: 155270-99-8, the structural formula is as follows. [0003] [0004] Parkinson's disease (PD) is a chronic progressive movement disorder common in the elderly. At present, although there are drugs that can slow down the symptoms of the disease and slow down the course of the disease, there is still a lack of effective preventive drugs. The current treatment of this disease is mainly based on dopamine replacement therapy, the most commonly used are dopamine-mim...

Claims

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Application Information

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IPC IPC(8): C07D473/06
Inventor 王长浩
Owner 南京瑞天医药科技有限公司
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