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Pregabalin production method

A production method, the technology of ibugaba, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of complex manufacturing process and high production cost, and achieve low manufacturing cost, simple manufacturing process and high output high effect

Inactive Publication Date: 2015-07-01
蒋学京
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the current process of producing ibugaba, the manufacturing process is complicated and the production cost is high

Method used

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Comparison scheme
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Embodiment Construction

[0006] Now in conjunction with the present invention for further detailed description.

[0007] A kind of production method of ibugaba of the present invention is characterized in that concrete steps are as follows: 3-cyano-5-methylhex-3-enoic acid ethyl ester and lithium hydroxide monohydrate are dissolved in tetrahydrofuran and water, Stir vigorously at room temperature for 4 hours, acidify with 3mol / L hydrochloric acid to pH 2, extract with ethyl acetate, combine the extracts, dry, concentrate under reduced pressure, dissolve the residue in ethyl acetate, add tert-butylamine in ethyl acetate solution, filter Collect the precipitate and dry it to get 3-cyano-5-methylhex-3-enoic acid tert-butylammonium salt. The ammonium salt and Rh(COD)BF4 are dissolved in methanol, at 27~33°C and 0.35MPa hydrogen pressure Stir overnight at low temperature, add to potassium hydroxide aqueous solution, concentrate under reduced pressure, add nickel A-7000 catalyst, stir overnight under 0.35MP...

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Abstract

The present invention relates to a pregabalin production method, which concretely comprises: dissolving 3-cyano-5-methyl-hex-3-olefinic acid ethyl ester and a lithium hydroxide monohydrate in tetrahydrofuran and water, carrying out acidification with 3 mol / L hydrochloric acid to achieve the pH value of 2, dissolving the residue in ethyl acetate, adding an ethyl acetate solution of tert-butylamine to obtain 3-cyano-5-methyl-hex-3-olefinic acid tert-butylamine salt, dissolving the 3-cyano-5-methyl-hex-3-olefinic acid tert-butylamine salt and Rh(COD)BF4 in methanol, adding a nickel A-7000 catalyst, stirring overnight under a hydrogen pressure of 0.35 MPa, filtering, washing the filter cake with methanol, mixing the filtrate and the washing, carrying out pressure reducing distillation to obtain the methanol, adding isopropanol, heating to a temperature of 65 DEG C, heated to a temperature of 73 DEG C, quenching to a temperature of 50 DEG C, slowly cooling to a room temperature, cooling to a temperature of 0-5 DEG C, maintaining for 3.5 h, filtering, washing the filter cake with isopropanol, and drying to obtain the pregabalin. The pregabalin production method of the present invention has characteristics of simple manufacturing process, low manufacturing cost, and high yield.

Description

technical field [0001] The invention relates to the field of medicine preparation, in particular to a production method of ibugaba. Background technique [0002] Ibugaba is one of the most promising epilepsy drugs under development, with better efficacy and more convenient administration. It can also be used to treat pain and anxiety. Because currently it is in the process of producing ibugaba, the manufacturing process is complicated and the production cost is high. Contents of the invention [0003] The technical problem to be solved by the present invention is: in order to overcome the above-mentioned problems, a production method of ibugaba is provided. [0004] The technical scheme adopted by the present invention to solve its technical problems is: a kind of production method of ibugaba, concrete steps are as follows: 3-cyano-5-methylhex-3-enoic acid ethyl ester and lithium hydroxide monohydrate The product was dissolved in tetrahydrofuran and water, stirred vigor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/08C07C227/10
Inventor 蒋学京
Owner 蒋学京