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A kind of method of multiphase duplex continuous production and preparation of vildagliptin

A complex, temperature-controlled technology, applied in organic chemistry and other fields, can solve problems such as energy consumption yield, reaction time follow-up treatment, etc., and achieve the effect of reducing follow-up treatment steps, shortening time, and low stirring requirements

Active Publication Date: 2022-07-19
CHINA MEHECO SANYANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the above problems, one of the objects of the present invention is to provide a method for the preparation of vildagliptin by multi-phase compound continuous production, so as to solve the problems of reaction on equipment requirements, energy consumption, yield, reaction time, follow-up treatment, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take L-prolineamide with a concentration of 40% as the starting material, add 2,6-lutidine, heat and stir to dissolve it, control the temperature to -30°C, and add it dropwise to a concentration of 50% of ethyl chloride In the acid chloride, react for 0.5h, the reaction solution is not treated, add dehydrating agent concentrated sulfuric acid, react for 0.5h, the reaction solution is quenched, and then use sodium bicarbonate to adjust its pH value to neutrality, take the organic layer by layer and add dropwise amantadine In the alcohol solution, the temperature is controlled at 0° C. and kept warm, concentrated, pulped with methyl tert-butyl ether or isopropanol solution, filtered, washed with filter cake, and dried to obtain vildagliptin.

Embodiment 2

[0026] The preparation process of Example 2 is the same as that of Example 1, except that the concentration of L-prolineamide is different.

[0027] Take L-prolineamide with a concentration of 60% as the starting material, add 2,6-lutidine, heat and stir to dissolve it, control the temperature to -30°C, and add it dropwise to a concentration of 50% of ethyl chloride In the acid chloride, react for 0.5h, the reaction solution is not treated, add dehydrating agent concentrated sulfuric acid, react for 0.5h, the reaction solution is quenched, and then use sodium bicarbonate to adjust its pH value to neutrality, take the organic layer by layer and add dropwise amantadine In the alcohol solution, the temperature is controlled at 0° C. and kept warm, concentrated, pulped with methyl tert-butyl ether or isopropanol solution, filtered, washed with filter cake, and dried to obtain vildagliptin.

Embodiment 3

[0029] The preparation process of Example 3 is the same as that of Example 1, except that the concentration of L-prolineamide is different.

[0030] Take L-prolineamide with a concentration of 80% as the starting material, add 2,6-lutidine, heat and stir to dissolve it, control the temperature to -30°C, and add it dropwise to a concentration of 50% of ethyl chloride In the acid chloride, react for 0.5h, the reaction solution is not treated, add dehydrating agent concentrated sulfuric acid, react for 0.5h, the reaction solution is quenched, and then use sodium bicarbonate to adjust its pH value to neutrality, take the organic layer by layer and add dropwise amantadine In the alcohol solution, the temperature is controlled at 0° C. and kept warm, concentrated, pulped with methyl tert-butyl ether or isopropanol solution, filtered, washed with filter cake, and dried to obtain vildagliptin.

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PUM

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Abstract

The invention discloses a method for preparing vildagliptin by multiphase duplex continuous production. In the acid chloride solution, the reaction is carried out, the reaction solution is not treated, a dehydrating agent is added, quenched, the pH value is adjusted to neutrality, the organic layer is layered and added dropwise to the amantadine alcohol solution, the temperature is controlled and kept warm, concentrated, pulped, and filtered. , washing the filter cake, and drying to obtain vildagliptin. In the present invention, 2,6-lutidine is also used as a solvent as an acid binding agent, and the addition of amantadine is carried out under homogeneous conditions without generating solids, and the reaction solution is directly used to carry out the next step reaction. The stirring requirement is low; while the post-processing steps are reduced, the energy consumption is reduced and the yield is improved; the commercial production can be more realized; the time is shortened, the post-processing is simple, and the operating conditions are simple.

Description

technical field [0001] The present invention relates to the field of preparation methods of vildagliptin. More specifically, the present invention relates to a method for preparing vildagliptin by multiphase duplex continuous production. Background technique [0002] The clinical drug vildagliptin is another orally administered dipeptidyl peptidase-IV (DPP-IV) inhibitor after sitagliptin. , was approved for marketing in the European Union in 2008 for the treatment of type 2 diabetes. Vildagliptin is a selective, competitive and reversible DPP24 inhibitor. [0003] But in general, the reaction route for synthesizing vildagliptin is long, the reaction is cumbersome, the reaction is carried out under two-phase conditions, and the production equipment is required to be high, so the energy consumption is large, the yield is low, the reaction time is long, and the follow-up treatment It is complicated and has high operating conditions, which is not conducive to the realization ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/16
CPCC07D207/16
Inventor 宋光文王玉娟陈海刚朱峰傅超婷
Owner CHINA MEHECO SANYANG PHARMA CO LTD
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