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Salfaprodil impurity B, and preparation method and application thereof

A technology of impurity and reaction, applied in the field of sofadil impurity B and its preparation, can solve the problems of reducing drug efficacy, increasing requirements, toxic and side effects, etc., to improve the quality of finished products, strengthen control, improve accurate positioning and qualitative effect

Active Publication Date: 2017-06-13
ZHEJIANG APELOA JIAYUAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Impurities contained in drugs generally reduce the efficacy of drugs, and even cause serious side effects in some cases. As people's health awareness is getting higher and higher, the requirements for the content of impurities in drugs are getting higher and higher.

Method used

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  • Salfaprodil impurity B, and preparation method and application thereof
  • Salfaprodil impurity B, and preparation method and application thereof
  • Salfaprodil impurity B, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The synthesis of embodiment 1 compound (Ⅲ)

[0043] Dissolve 42.13g of compound (II) in 210mL of water, lower the temperature to 0-10°C, add hydrochloric acid thereto, adjust the pH to 2-4, and stir at room temperature for half an hour. Extracted three times with ethyl acetate, combined the organic phases, washed once with saturated brine, dried over anhydrous sodium sulfate; filtered to remove sodium sulfate, and concentrated the filtrate under reduced pressure to obtain 38.1 g of compound (Ⅲ), yield 99%, HPLC purity 100% . The reaction formula is as follows:

[0044]

Embodiment 2

[0045] The synthesis of embodiment 2 compound (Ⅲ)

[0046] Dissolve 42.13g of compound (II) in 210mL of water, lower the temperature to 0-10°C, add hydrochloric acid thereto, adjust the pH to 2-4, and stir at room temperature for half an hour. Extracted three times with isopropyl acetate, combined the organic phases, washed once with saturated brine, dried over anhydrous sodium sulfate; filtered to remove sodium sulfate, and concentrated the filtrate under reduced pressure to obtain 37.2 g of compound (Ⅲ), yield 97%, HPLC purity 100 %.

Embodiment 3

[0047] The synthesis of embodiment 3 compound (I)

[0048] 38.1g of the compound (Ⅲ) prepared in Example 1 was dissolved in 250mL of methanol, and 3.8g of 5% palladium carbon and 13.8g of anhydrous potassium carbonate were added thereto; the reaction kettle was first replaced with nitrogen three times, and then replaced with hydrogen After three times, control the pressure to 1.0-2.0Mpa and react at a temperature of 40-50°C. After reacting for 8 hours, samples were taken for HPLC detection, and the reaction was stopped if the raw material content was less than or equal to 5%. The reaction solution was filtered to remove palladium carbon, and the filtrate was concentrated under reduced pressure to remove methanol. Add 100 mL of water to the concentrate, and adjust the pH to 2-4 with hydrochloric acid. Extracted three times with ethyl acetate, combined the organic phases, washed once with saturated brine, and dried over anhydrous sodium sulfate; the sodium sulfate was removed ...

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Abstract

The invention discloses a salfaprodil impurity B, and a preparation method and application thereof, belonging to the field of pharmaceutical and chemical industry. The structure of the salfaprodil impurity B is disclosed as Formula (I), and the salfaprodil impurity B is not reported in the documents currently. The preparation method of the salfaprodil impurity B comprises the following step: by using salfaprodil as the raw material, carrying out acidification and reduction to obtain the impurity B. The synthesis of the salfaprodil impurity B provides a qualified reference substance for quality control on salfaprodil.

Description

technical field [0001] The invention relates to an impurity of sofadil, a medicine for treating and preventing acute and chronic neurodegenerative diseases of the central nervous system, and a preparation method thereof, in particular to a sofadil impurity B, a preparation method and application thereof, belonging to the field of medicine and chemical industry . Background technique [0002] Sofaprodil (Salfaprodil), the chemical name is 2-hydroxy-5-{[2,3,5,6-tetrafluoro-4-(trifluoromethyl)benzyl]amino}benzoate potassium, and its structural formula is as follows Shown: [0003] [0004] Sofadil is a moderately potent N-methyl-D-aspartate (NMDA) receptor antagonist and a potent antioxidant with dual neuroprotective effects, simultaneously blocking NMDA receptors It mediates excitotoxicity and the body's oxidative stress response, and its protective effect on neurological function can last for more than 28 days, providing a wide range of neuroprotective effects and expand...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/16C07C229/64G01N30/02
CPCC07C227/16C07C227/18C07C229/64G01N30/02
Inventor 赫亚征杨浦生胡明阳吴瑜亮周雄飞雷江
Owner ZHEJIANG APELOA JIAYUAN PHARMA
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