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Purification method for preparing high-purity perampanel intermediate

A technology of intermediates and refining methods, which is applied in the field of refining perampanel intermediates, and can solve the problems of expensive benzonitrile intermediates, many synthesis steps, and high costs

Pending Publication Date: 2022-08-05
BEIJING VENTUREPHARM BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Because the preparation of 2-(5-acetyl-2-oxo-1-phenyl-1,2-dihydropyridin-3-yl)benzonitrile intermediate is expensive and the number of synthesis steps is many, it is necessary to find an efficient Purification of 2-(5-acetyl-2-oxo-1-phenyl-1,2-dihydropyridin-3-yl)benzonitrile The reaction conditions of crude benzonitrile solution are critical for industrial production
At present, the method used according to the patent CN103980188B_CN is to use heptane or column chromatography to purify, but the cost is relatively high

Method used

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  • Purification method for preparing high-purity perampanel intermediate
  • Purification method for preparing high-purity perampanel intermediate
  • Purification method for preparing high-purity perampanel intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 50 ml of freshly prepared 2-(5-acetyl-2-oxo-1-phenyl-1,2-dihydropyridin-3-yl) benzonitrile crude DMF solution to 80 ml in a ratio of 10:15 acetic acid In the ethyl ester-petroleum ether solution, heat to 50 °C for 1 hour, filter while hot, stir and crystallize, control the temperature to 20-25 °C for crystallization for 5 hours, and obtain refined products after suction filtration and drying. The chemical purity is 99.1%, the maximum Single miscellaneous 0.06%.

Embodiment 2

[0015] Add 10 ml of freshly prepared 2-(5-acetyl-2-oxo-1-phenyl-1,2-dihydropyridin-3-yl) benzonitrile crude DMF solution to 16 ml in a ratio of 5:15 acetic acid In the ethyl ester-petroleum ether solution, heat to 50 °C for 1 hour, filter while hot, stir and crystallize, control the temperature to 20-25 °C for crystallization for 5 hours, and obtain refined products after suction filtration and drying. The chemical purity is 98.1%, the maximum Single miscellaneous 0.08%.

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Abstract

The invention relates to a method for refining a perampanel intermediate, in particular to a method for refining 2-(5-acetyl-2-oxo-1-phenyl-1, 2-dihydropyridine-3-yl) benzonitrile. The method is characterized in that a refined product is prepared by using an ethyl acetate-petroleum ether mixed solution through a recrystallization method. Compared with traditional purification methods such as column chromatography, freeze-drying and the like, the method has the advantages of convenience, rapidness, suitability for industrial production and the like.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and relates to a method for purifying a perampanel intermediate. Background technique [0002] Perampanel was approved by the U.S. Food and Drug Administration (FDA) on October 22, 2012 for the adjuvant treatment of epilepsy. Perampanel is currently approved for focal generalized epilepsy with or without secondary generalized epilepsy in patients 12 years of age or older in more than 55 countries including Australia, North America, Europe, Asia and Russia Adjunctive treatment of epilepsy. Perampanel is also approved as adjunctive therapy for primary generalized tonic-clonic (PGTC) seizures in patients over 12 years of age in North America, Europe, Asia, and Russia. Studies and clinical evidence in preclinical epilepsy models suggest that perampanel has antiepileptic potential and is effective in patients with or without secondary generalization, primary generalized seizures, and other focal s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/64
CPCC07D213/64
Inventor 张晓雷罗米海宋雪梅
Owner BEIJING VENTUREPHARM BIOTECH