Barnidipine hydrochloride synthesis process

A technology of barnidipine hydrochloride and synthesis process, applied in directions such as organic chemistry, can solve problems such as low production efficiency, complex production process, low separation efficiency, etc., and achieve the effects of improving utilization rate, overcoming many processes, and improving work efficiency

Inactive Publication Date: 2016-05-04
赵建英
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the current synthesis process of barnidipine hydrochloride, the process flow is not easy to implement, the separation efficiency i

Method used

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Examples

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Embodiment

[0015] The synthesis process of barnidipine hydrochloride in this embodiment includes the following steps:

[0016] (1) 3-Hydroxypropionitrile (I) and diketene (II) are reacted in the presence of an organic base catalyst at a reaction temperature of 10°C, preferably 90°C, and a reaction time of 72h, preferably 3, to obtain compound (VI) ;

[0017] (2) The above compound (VI) reacts with m-nitrobenzaldehyde (III) in the presence of a protic or aprotic solvent, the reaction temperature is 5°C, preferably 70°C, and the reaction time is 72h, preferably 24h. Compound (VII);

[0018] (3) The above compound compound (VII) is reacted with ethyl β-aminocrotonate (IV) in a protic or aprotic solvent, the reaction temperature is 150°C, preferably 30°C, and the reaction time is 72h, preferably 1h, Compound (VIII) can be obtained;

[0019] "(4) The above compound compound (VIII) is hydrolyzed by a strong base in a protic or aprotic solvent, the reaction temperature is 150°C, preferably 70°C, and ...

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Abstract

The present invention discloses a barnidipine hydrochloride synthesis process, which comprises that: (1) 3-hydroxy propionitrile (I) and diketene (II) are subjected to a reaction to obtain a compound (VI); (2) the compound (VI) and m-nitrobenzaldehyde (III) are subjected to a reaction to obtain a compound (VII); (3) the compound (VII) and ethyl beta-aminocrotonate (IV) are subjected to a reaction to obtain a compound (VIII); (4) the compound (VIII) is subjected to hydrolysis with a strong base to obtain a compound (IX); (6) the compound (IX) is split with a chiral organic base to obtain a compound (X); (6) the compound (X) and benzyl pyrrole alcohol (V) are subjected to a reaction to obtain a compound (XI); and (7) the compound (XI) is added to a hydrogen chloride solution so as to obtain the barnidipine hydrochloride (XII). According to the present invention, the synthesis process has the following advantages that: (1) the reaction conditions are mild, and the products of every step are easy to separate and purify, and have controlled quality; (2) the yields of each step are high, the used raw materials and the used auxiliary materials are easy to obtain, and the total cost is low; and (3) the column separation is not required, and the process is suitable for industrial production.

Description

Technical field [0001] The invention belongs to the field of chemical processes, and specifically relates to a synthesis process of barnidipine hydrochloride. Background technique [0002] The synthesis process of barnidipine hydrochloride includes at least basic processes such as separation, purification, and reflux. In the current synthesis process of barnidipine hydrochloride, the process flow is not easy to implement, the separation efficiency is low, the recycling of raw materials cannot be realized, the production process is complicated, and the production efficiency is low. Summary of the invention [0003] In order to overcome the above-mentioned technical problems in the prior art, the purpose of the present invention is to provide a synthesis process of barnidipine hydrochloride. The present invention not only has a simple production process, improves work efficiency, but also realizes product quality assurance. [0004] The synthesis process of barnidipine hydrochlorid...

Claims

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Application Information

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IPC IPC(8): C07D401/12
Inventor 赵建英
Owner 赵建英
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