A kind of method for preparing midanaxin

A midanaxine and route technology, applied in the field of preparation of midanaxine, can solve the problems of low safety, unfriendly human body and environment, blindness, etc., and achieve the effect of being friendly to human body and environment

Active Publication Date: 2016-01-13
JIANGZI QINGFENG PHARMACEUTICALS INC
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] Hydrogen peroxide solution is used in this method, but hydrogen peroxide solution has strong oxidizing properties and is corrosive to a certain extent. Inhalation of the vapor or mist is highly irritating to the respiratory tract, and direct contact with the liquid can cause irreversible damage or even blindness, which is safe. Non-toxic, unfriendly to human body and environment

Method used

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  • A kind of method for preparing midanaxin
  • A kind of method for preparing midanaxin
  • A kind of method for preparing midanaxin

Examples

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Effect test

Embodiment 1

[0029] Embodiment 1: Preparation of 4-bromo-2,2-diphenylbutyronitrile

[0030] Add 400mL dry tetrahydrofuran to a 2L reaction flask, add 60% sodium hydride (82.8g, 2.06mol) under nitrogen protection, and stir to obtain gray cloudy liquid A. Fully dissolve diphenylacetonitrile (200g, 1.04mol) and 1,2-dibromoethane (204.2g, 1.08mol) with 400mL dry tetrahydrofuran solution to obtain a colorless clear liquid B; Drop B into the turbid solution A, and keep it warm at 10-15°C for 6 hours. After the reaction is detected by TLC, add a small amount of water dropwise to the reaction system until no bubbles are generated. Then add 800mL of water and 400mL of ethyl acetate, stir, separate the layers, wash the organic layer with water and saturated sodium chloride solution, dry the organic layer with anhydrous sodium sulfate, filter with suction, and concentrate under reduced pressure to obtain 310g of yellow liquid.

[0031] The obtained yellow liquid was stirred and dissolved with 800 mL...

Embodiment 2

[0032] Embodiment 2: Preparation of 4-bromo-2,2-diphenylbutanamide

[0033] Add 4-bromo-2,2-diphenylbutyronitrile (150g, 0.5mol), 750mL 6mol / L KOH solution, 750mL dimethyl sulfoxide into a 3L reaction flask, heat to 100-120°C and stir for reaction for 1 hour. After the TLC detection reaction is completed, cool down to 40°C, add 2000mL of water and 2000mL of dichloromethane, stir, separate the layers, wash the organic layer with water, saturated sodium bicarbonate and sodium chloride solution, separate the layers, and dry the organic layer with anhydrous sodium sulfate , suction filtration, and concentration under reduced pressure to obtain 161.92 g of brown oily liquid, with a yield of 96%.

Embodiment 3

[0034] Embodiment 3: Preparation of 4-bromo-2,2-diphenylbutanamide

[0035] Add 4-bromo-2,2-diphenylbutyronitrile (150g, 0.5mol), 666mL6mol / L NaOH solution, 750mL dimethyl sulfoxide into a 3L reaction flask, heat to 100-120°C and stir for reaction for 1h. After the TLC detection reaction is completed, cool down to 40°C, add 2000mL of water and 2000mL of dichloromethane, stir, separate the layers, wash the organic layer with water, saturated sodium bicarbonate and sodium chloride solution, separate the layers, and dry the organic layer with anhydrous sodium sulfate , suction filtration, and concentration under reduced pressure to obtain 146.73 g of brown oily liquid with a yield of 87%.

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Abstract

The invention discloses a method for preparing imidafenacin. The method comprises the steps of hydrolyzing 4-bromo-2,2-diphenyl butyronitrile into acid amide under an alkaline condition, and then enabling the acid amide to react with 2-methylimidazole so as to obtain a target product. The preparation method provided by the invention is high in yield, economical, simple, convenient, friendly to human body and environment, and suitable for industrialized large-scale production.

Description

technical field [0001] The invention belongs to the field of drug synthesis, and in particular relates to a new method for preparing midanacin. Background technique [0002] Overactive bladder syndrome (symptomatic overactive bladder, OAB) is a common chronic lower urinary tract dysfunction, the International Anti-Urinary Incontinence Society (ICS) defined it as a urinary urgency (a strong sense of urination), frequency and urgent A syndrome characterized by sexual urinary incontinence. [0003] The incidence rate of OAB is relatively high. The incidence rate of men over 75 years old in European and American countries is as high as 42%, and the incidence rate of women is slightly lower at 31%. The incidence rate of men over 50 years old in Beijing in China is as high as 16.4%. The overall incidence of incontinence and urge incontinence is 40.4%, which seriously affects the physical and mental health of patients and reduces the quality of life. There is no specific treatmen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/56
CPCC07D233/56
Inventor 谢宁杨小玲蔡鸿飞邵秀芬程帆付敏熊先水沈曦何党军崔刚
Owner JIANGZI QINGFENG PHARMACEUTICALS INC
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