Istradefylline raw material drug and preparation method thereof

A technology of istraphylline and bulk drug, applied in the field of istraphylline bulk drug and preparation thereof, can solve the problems of not effectively reducing or avoiding the side effects of istraphylline and the like

Active Publication Date: 2018-11-23
JIANGSU HENGRUI MEDICINE CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, this product still contains the compound of formula III, and its quality control measures have not effectively reduced or avoided the side effects of istradefylline. Ther...

Method used

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  • Istradefylline raw material drug and preparation method thereof
  • Istradefylline raw material drug and preparation method thereof
  • Istradefylline raw material drug and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach

[0056] The following examples are used to further describe the present invention, but these examples do not limit the scope of the present invention.

[0057] The experimental methods not indicating specific conditions in the examples of the present invention are generally in accordance with conventional conditions, or in accordance with the conditions suggested by raw material or commodity manufacturers. Reagents without specific sources indicated are conventional reagents purchased in the market.

Embodiment 1

[0058] Example 1, E-N-(6-amino-1,3-diethyl-2,4-dione-1,2,3,4-tetrahydropyrimidin-5-yl)-3-(3,4- Preparation of dimethoxy) propionamide (compound A)

[0059]

[0060] Suspend the compound 1,3-diethyl-5,6-diaminouracil (1.0kg, prepared according to the method of EP0590919A1) of formula 1 in dichloromethane, add pyridine (1.6kg) under stirring, dissolve the dichloro Compound 2 (1.54kg) in methane (3.5L) was added dropwise to the reaction system, and the dropwise addition was completed in about 1.5 hours. After stirring at room temperature for 15-20 hours, a saturated aqueous sodium bicarbonate solution was added dropwise to the reaction solution to adjust the pH to Around 7-8, solids are precipitated. After filtration, the filter cake was washed twice with water, and the filter cake was dried to obtain a light yellow powdery solid product (1.56 kg), with a yield of 79.5%.

Embodiment 2

[0061] Example 2. Preparation of 8-((E)-2-(3,4-dimethoxyphenyl)vinyl)-1,3-diethyl-3,7-dihydro-1H-purine-2 , the preparation of 6-diketone (compound of formula I)

[0062]

[0063] Method A:

[0064] Formula A compound (500g, 1.29mol) was added in 10L reactor, then added isopropanol (2.5L), stirred, sodium hydroxide solid (486g, 12.15mol) was dissolved in water (2.0L), then stirred Add it dropwise to the reaction system quickly, and the dropwise addition is completed in about 30 minutes. The temperature of the reaction is raised to 75-80°C. After 8-9 hours of reaction, TLC monitors that the raw materials have reacted completely, and the reaction solution is cooled to below 20°C, and then heated with 6M Hydrochloric acid was used to adjust the pH of the reaction system to 3-4, and a solid was precipitated. After filtering, the resulting filter cake was washed once with a small amount of water, and dried to obtain a light yellow-green powder product (383 g), with an HPLC pur...

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PUM

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Abstract

The invention relates to an istradefylline raw material drug and a preparation method thereof. Specifically, the invention relates to an istradefylline raw material drug. A compound shown in formula III is not higher than 0.5% and is a medicine preparation consisting of the istradefylline raw material drug and a pharmacologically acceptable carrier and/ or diluent. The raw material drug and the preparation thereof have better safety, effectiveness and stability. The formula III is shown in the description.

Description

technical field [0001] The invention relates to a raw material drug of istradefylline and a preparation method thereof. Background technique [0002] Itradefylline (Istradefylline, KW-6002, ) is an oral adenosine A2a receptor antagonist developed by Kyowa Hakko Kirin, a non-dopamine compound. It improves the motor function of Parkinson's patients by changing the activity of neurons, and can improve the initial stage of Parkinson's patients. At the same time, it has brought a turning point in the treatment of patients with advanced Parkinson's disease, and proved that it can affect other neurotransmitters, and non-dopamine drugs can benefit patients with advanced Parkinson's disease; it is compatible with levodopa products (L-DOPA) Combined use in patients with Parkinson's disease to improve the symptoms of diminished efficacy, and can also reduce the amount of levodopa, thereby preventing or delaying the occurrence of dyskinesia. [0003] In order to reduce or avoid the a...

Claims

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Application Information

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IPC IPC(8): C07D473/06A61K31/522A61P25/14A61P25/16
CPCA61P25/14A61P25/16C07D473/06
Inventor 李长松南文汇孙绍光薛州洋
Owner JIANGSU HENGRUI MEDICINE CO LTD
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