A kind of preparation method of istradefylline impurity standard substance

A technology of istradefylline and standard products, applied in the field of medicine, can solve the problems of cumbersome operation, low yield, large light surface, etc., and achieve an effect that is extremely easy to achieve

Active Publication Date: 2018-09-18
HEFEI JIUNUO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires istradefylline to be made into microparticles and spread on the panel. The light surface is large, the operation is cumbersome, and the yield is low (60%), which is only suitable for laboratory micro-preparation.

Method used

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  • A kind of preparation method of istradefylline impurity standard substance
  • A kind of preparation method of istradefylline impurity standard substance
  • A kind of preparation method of istradefylline impurity standard substance

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Effect test

Embodiment 1

[0040] The preparation method of istradefylline impurity standard substance in the present embodiment is as follows:

[0041] 1. Under the protection of nitrogen, put 200ml of chloroform, 3.5g (26mmol) of aluminum trichloride and 10g (26mmol) of istradefylline into a 500ml colorless glass reaction bottle in sequence, and stir at 30-40°C until completely dissolved , the reaction bottle was tightly closed, placed under a 254nm ultraviolet lamp for 10 hours, and the temperature was controlled at 35-40°C; after the reaction, the reaction solution was washed with 200ml of water and 200ml of saturated aqueous sodium chloride solution, and the organic layer was concentrated to dryness at 30-40°C under reduced pressure. , 9.4 g of impurity crude product was obtained, with a yield of 94.0%.

[0042] 2. Add 100ml of dichloromethane to 9.4g of crude impurities, heat and stir at 30-35°C to dissolve, filter while hot, add 500ml of ethanol to the filtrate, stir and crystallize at 0-10°C for...

Embodiment 2

[0053] The preparation method of istradefylline impurity standard substance in the present embodiment is as follows:

[0054] 1. Under the protection of nitrogen, put 500ml of chloroform, 14g (104mmol) of aluminum trichloride and 20g (52mmol) of istradefylline into a 1L colorless glass reaction bottle successively, stir at 30-40°C until completely dissolved, Seal the reaction bottle, place it under a 254nm ultraviolet lamp for 12 hours, and control the temperature at 35-40°C; after the reaction, the reaction solution is washed with 500ml of water and 500ml of saturated aqueous sodium chloride solution, and the organic layer is concentrated to dryness at 30-40°C under reduced pressure. 18.3 g of impurity crude product was obtained with a yield of 91.5%.

[0055] 2. Add 250ml of dichloromethane to 18.3g of crude impurities, heat and stir at 30-35°C to dissolve, filter while hot, add 2000ml of ethanol to the filtrate, stir and crystallize at 0-10°C for 2h, filter, and wash the fi...

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Abstract

The invention discloses a preparation method of an istradefylline impurity standard. Istradefylline is subjected as a raw material to Lewis acid catalysis [2+2] cycloaddition, the reaction product is then refined to obtain pure 8,8'-((1R,2R,3S,4S)-2,4-bis(3,4-dimethoxyphenyl)cyclobutane-1,3-diyl)bis(1,3-diethyl-7-methyl-1H-purine-2,6(3H,7H)-dione), and the content of the pure product is calibrated by conventional analytic means. The preparation method provided herein is simple and has a short preparation cycle, and the calibrated content is higher than 99.0%. Istradefylline impurity provided herein may act as an impurity standard, applied to the qualitative and quantitative study and detection on istradefylline material and its preparation impurities.

Description

1. Technical field [0001] The invention relates to a preparation method of a drug impurity standard product, in particular to a preparation method of an istradefylline impurity standard product, and belongs to the technical field of medicine. 2. Background technology [0002] Itradefylline, the chemical name is (E)-8-(3,4-dimethoxystyryl)-1,3-diethyl-7-methyl-3,7-dihydro -1H-purine-2,6-dione, a selective adenosine A 2 A receptor antagonist, developed by Japan Kyowa Hakko Kirin Company. Itraphylline Tablets (trade name Nouriast, specification 20mg) was approved for marketing by PMDA in Japan in March 2013. It is clinically used to treat Parkinson's disease and improve the dyskinesia in the early stage of Parkinson's syndrome. End-of-dose phenomenon due to treatment. [0003] During the synthesis and storage of istradefylline raw materials and its preparations, there will be degradation impurities: 8,8'-((1R,2R,3S,4S)-2,4-bis(3,4-dimethoxybenzene Base) cyclobutane-1,3-diyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D519/00
CPCC07D519/00
Inventor 吴标佘文龙凌林
Owner HEFEI JIUNUO MEDICAL TECH
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