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Preparation method of chlocibutamine

A kind of technology of chlornamonamide and sec-butylamine, which is applied in the field of preparation of chlornamonamide, and can solve the problems such as the preparation method of compounds that have not yet been seen

Inactive Publication Date: 2010-09-22
WEIHAI DISU PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on the preparation method of its compound

Method used

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  • Preparation method of chlocibutamine
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  • Preparation method of chlocibutamine

Examples

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Embodiment 1

[0023] Preparation of 3,4-dichlorophenylacrylic acid

[0024] 2.5kg (14.28 moles) of 4-dichlorobenzaldehyde, 1.41kg (14.36 moles) of potassium acetate, 3.96kg (38.82 moles) of acetic anhydride, pyridine 0.19 kg (2.45 moles). 138 ~ 142 ℃ heat preservation reaction. After the reaction was completed, the reaction solution was slowly poured into 18 liters of water, stirred while pouring, cooled to 25°C with stirring, filtered under reduced pressure, washed with water, and dried to obtain crude 3,4-dichlorophenylacrylic acid.

[0025] Put the crude product of 3,4-dichlorophenylacrylic acid into the reactor, add 12 liters of water and 1.7 liters of concentrated ammonia water, heat and stir to dissolve. Add 0.2 kg of activated carbon and stir at 95°C for 1 hour. Filtrate hot, add concentrated hydrochloric acid to the filtrate in portions under stirring, control the pH at 2.0-2.5, a large amount of white precipitate precipitates, stir and cool down to 17°C. It was filtered under r...

Embodiment 2

[0031] Preparation of 3,4-dichlorophenylacrylic acid

[0032] In 10 liters of glass reactors with stirring and reflux, add 3,4-dichlorobenzaldehyde 2.5kg (14.28 moles) respectively, potassium acetate 1.68kg (17.14 moles), acetic anhydride 3.68kg (36.0 moles), Pyridine 0.169kg (2.61 moles). 135 ~ 138 ℃ insulation for 6 hours. The reaction solution was slowly poured into a stainless steel bucket filled with 16 liters of water, and stirred while pouring. A large amount of yellow precipitate was precipitated, stirred and cooled to 25°C, filtered under reduced pressure, washed with water, and dried to obtain 3,4-dichlorophenylacrylic acid.

[0033] Put the crude product of 3,4-dichlorophenylacrylic acid into the reactor, add 12 liters of water and 1.7 liters of concentrated ammonia water, heat and stir to dissolve. Add 0.2 kg of activated carbon and stir at 95°C for 1 hour. Filtrate hot, add concentrated hydrochloric acid to the filtrate in portions under stirring, control the ...

Embodiment 3

[0039] Preparation of 3,4-dichlorophenylacrylic acid

[0040] In 10 liters of glass reactors with stirring and reflux, add 3,4-dichlorobenzaldehyde 2.5kg (14.28 moles) respectively, potassium acetate 1.68kg (17.14 moles), acetic anhydride 3.64kg (35.7 moles), Pyridine 0.28kg (3.57 moles). Keep warm at 143-145°C. The reaction solution was slowly poured into a stainless steel bucket filled with 18 liters of water, and stirred while pouring. A large amount of yellow precipitate was precipitated, stirred and cooled to 25°C, filtered under reduced pressure, washed with water, and dried to obtain 3,4-dichlorophenylacrylic acid.

[0041] Put the crude product of 3,4-dichlorophenylacrylic acid into the reactor, add 10 liters of water and 1.5 liters of concentrated ammonia water, heat and stir to dissolve. Add 0.2 kg of activated carbon and stir at 95°C for 1 hour. Filtrate hot, add concentrated hydrochloric acid to the filtrate in portions under stirring, control the pH at 2.0-2.5...

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Abstract

The invention relates a preparation method of chlocibutamine, which is characterized by comprising the following steps: 1. reacting 3, 4-dichlorobenzaldehyde serving as a starting material with acetic anhydride and potassium acetate to obtain 3, 4-dichlorobenzene crylic acid; 2. reacting the 3, 4-dichlorobenzene crylic acid with thionyl chloride to obtain 3, 4-dichorophenyl acryloyl chloride; and 3. reacting the 3, 4-dichorophenyl acryloyl chloride with sec-butylamine to obtain the chlocibutamine.

Description

technical field [0001] The invention relates to a preparation method of clonamidine. Background technique [0002] Chlorocinamide is an aromatic acrylamide derivative, which is the abbreviation of 3,4-dichlorocinnamic acid butylamine, and its chemical name is: (1S,1R)-(E)-3-(3,4 -dichlorophenyl)-N-(1-methylpropyl)-2-acrylamide. [0003] This compound belongs to an innovative cinnamon amide derivative. Animal experiments have proved that it has a strong anti-epileptic effect and has pharmacological characteristics of low toxicity. For details, please refer to "Journal of Baotou Medical College" 2005 Volume 21 No. 4 In the period, the effect of chloramidine on the content of CYP450 in mice and the binding rate to plasma protein in rats. At present, there is no report on the preparation method of its compound. Contents of the invention [0004] The technical problem to be solved in the present invention is to provide a preparation method of chlorinated amine. [0005] The...

Claims

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Application Information

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IPC IPC(8): C07C233/11C07C231/02
Inventor 鞠传平高永吉邹元华刘炳朋李宗文于忠文
Owner WEIHAI DISU PHARMA CO LTD
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