Preparation method of chlocibutamine

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

Inactive Publication Date: 2012-11-21
WEIHAI DISU PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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
  • Preparation method of chlocibutamine
  • 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 3,4-dichlorobenzaldehyde, 1.41kg (14.36 moles) of potassium acetate, 3.96kg (38.82 moles) of acetic anhydride, 3.96kg (38.82 moles) of acetic anhydride, pyridine 0.19 kg (2.45 moles). The reaction was incubated at 138-142°C. 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, the solid portion was washed with water, and filtered to dryness to obtain crude 3,4-dichlorophenylacrylic acid.

[0025] The crude 3,4-dichlorophenylacrylic acid was put into the reactor, 12 liters of water and 1.7 liters of concentrated ammonia water were added, and the mixture was heated and stirred to dissolve. Add 0.2 kg of activated carbon and stir at 95°C for 1 hour. Hot filtration, adding concentrated hydrochloric acid to the filtrate in stages under stirring, controlling the pH...

Embodiment 2

[0031] Preparation of 3,4-dichlorophenylacrylic acid

[0032] In a 10-liter glass reactor with a stirring and refluxing device, 2.5kg (14.28 moles) of 3,4-dichlorobenzaldehyde, 1.68kg (17.14 moles) of potassium acetate and 3.68kg (36.0 moles) of acetic anhydride were added, respectively. Pyridine 0.169 kg (2.61 moles). Incubate at 135-138°C 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, which was stirred and cooled to 25° C., filtered under reduced pressure, washed with water, and filtered to dryness to obtain 3,4-dichlorophenylacrylic acid.

[0033] The crude 3,4-dichlorophenylacrylic acid was put into the reactor, 12 liters of water and 1.7 liters of concentrated ammonia water were added, and the mixture was heated and stirred to dissolve. Add 0.2 kg of activated carbon and stir at 95°C for 1 hour. Hot filtration, adding co...

Embodiment 3

[0039] Preparation of 3,4-dichlorophenylacrylic acid

[0040] In a 10-liter glass reactor with a stirring and refluxing device, 2.5kg (14.28 moles) of 3,4-dichlorobenzaldehyde, 1.68kg (17.14 moles) of potassium acetate, and 3.64kg (35.7 moles) of acetic anhydride were added, respectively. Pyridine 0.28 kg (3.57 moles). 143 ~ 145 ℃ insulation. 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, which was stirred and cooled to 25° C., filtered under reduced pressure, washed with water, and filtered to dryness to obtain 3,4-dichlorophenylacrylic acid.

[0041] The crude 3,4-dichlorophenylacrylic acid was put into the reactor, 10 liters of water and 1.5 liters of concentrated ammonia water were added, and the mixture was heated and stirred to dissolve. Add 0.2 kg of activated carbon and stir at 95°C for 1 hour. Hot filtration, adding concentrated ...

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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; and3. reacting the 3, 4-dichorophenyl acryloyl chloride with sec-butylamine to obtain the chlocibutamine.

Description

technical field [0001] The present invention relates to a preparation method of chlornamuramide. Background technique [0002] Chlorobutylamine is an aromatic acrylamide derivative, which is the abbreviated name of 3,4-dichlorocinnamamide, and its chemical name is: (1S,1R)-(E)-3-(3,4 -Dichlorophenyl)-N-(1-methylpropyl)-2-acrylamide. [0003] The compound belongs to an innovative cinnamamide derivative. Animal experiments have shown that it has strong anti-epileptic effect and has the pharmacological characteristics of low toxicity. For details, please refer to "Journal of Baotou Medical College", Vol. 21, No. 4, 2005 The effect of clonamide on CYP450 content in mice and its binding rate to plasma protein in rats. At present, there is no report on the preparation method of its compound. SUMMARY OF THE INVENTION [0004] The technical problem to be solved by the present invention is to provide a preparation method of chlornamonamide. [0005] The purpose of this inventio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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