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Method for multiphase compound continuous production and preparation of vildagliptin

A complex, temperature-controlled technology, applied in organic chemistry, etc., can solve the problems of long reaction time, cumbersome reaction, high operating conditions, etc., and achieve the effect of reducing subsequent processing steps, simple subsequent processing, and simple operating conditions

Active Publication Date: 2021-06-11
CHINA MEHECO SANYANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, usually the reaction route for synthesizing vildagliptin is long and the reaction is relatively tedious. The reaction is carried out under two-phase conditions, which requires high production equipment, so energy consumption is large, the yield is low, and the reaction time is long. Subsequent processing Complex, high operating conditions, not conducive to the realization of industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Using L-prolineamide with a concentration of 40% as the starting material, add 2,6-lutidine, heat and stir to dissolve it, control the temperature at -30°C, and add it dropwise to ethyl chloride with a concentration of 50%. In 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, then use sodium bicarbonate to adjust its pH value to neutral, take the organic layer by layer and add dropwise amantadine In the alcohol solution, control the temperature at 0°C and keep it warm, concentrate, beat with methyl tert-butyl ether or isopropanol solution, filter, wash the filter cake, and dry 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-prolinamide is different.

[0027] Using L-prolineamide with a concentration of 60% as the starting material, add 2,6-lutidine, heat and stir to dissolve it, control the temperature at -30°C, and add it dropwise to ethyl chloride with a concentration of 50%. In 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, then use sodium bicarbonate to adjust its pH value to neutral, take the organic layer by layer and add dropwise amantadine In the alcohol solution, control the temperature at 0°C and keep it warm, concentrate, beat with methyl tert-butyl ether or isopropanol solution, filter, wash the filter cake, and dry 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-prolinamide is different.

[0030] Using L-prolineamide with a concentration of 80% as the starting material, add 2,6-lutidine, heat and stir to dissolve it, control the temperature at -30°C, and add it dropwise to ethyl chloride with a concentration of 50%. In 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, then use sodium bicarbonate to adjust its pH value to neutral, take the organic layer by layer and add dropwise amantadine In the alcohol solution, control the temperature at 0°C and keep it warm, concentrate, beat with methyl tert-butyl ether or isopropanol solution, filter, wash the filter cake, and dry to obtain vildagliptin.

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PUM

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Abstract

The invention discloses a method for multiphase compound continuous production of vildagliptin, which comprises the following steps: adding a solvent into L-prolinamide, conducting heating and stirring to dissolve the L-prolinamide, controlling the temperature, dropwise adding a formed solution into a chloroacetyl chloride solution, conducting reacting, without treating the reaction solution, adding a dehydrating agent, conducting quenching, and adjusting the pH value to a neutral state, conducting layering, taking an organic layer, dropwise adding the organic layer into an amantadine alcohol solution, controlling the temperature, preserving heat, conducting concentrating, pulping and filtering, washing a filter cake, and conducting drying to obtain vildagliptin. According to the method, 2,6-dimethyl pyridine is used as a solvent and an acid-binding agent, amantadine alcohol is added under the homogeneous condition, no solid is generated, reaction liquid is directly adopted for next-step reaction, and the requirement for stirring of production equipment is low; the steps of post-treatment are reduced, the energy consumption is reduced, and the yield is improved; commercialized production can be realized; and the time is shortened, the post-treatment is simple, and the operation conditions are simple.

Description

technical field [0001] The invention relates to the field of preparation methods of vildagliptin. More specifically, the present invention relates to a method for preparing vildagliptin through multi-phase compound continuous production. Background technique [0002] Vildagliptin (vildagliptin) is another oral dipeptidyl peptidase-IV (DPP-IV) inhibitor after sitagliptin (sitagliptin), manufactured by Swiss Novartis Pharmaceutical Co., Ltd. , which was approved to be marketed in the EU in 2008 for the treatment of type 2 diabetes. Vildagliptin is a selective, competitive and reversible DPP24 inhibitor. [0003] However, usually the reaction route for synthesizing vildagliptin is long and the reaction is relatively tedious. The reaction is carried out under two-phase conditions, which requires high production equipment, so energy consumption is large, the yield is low, and the reaction time is long. Subsequent processing Complicated, high operating conditions, unfavorable f...

Claims

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Application Information

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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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