Method and device for continuous preparation of Vildagliptin by tubular reaction

A tubular reaction and tubular reactor technology, applied in the direction of organic chemistry, can solve the problems of long synthetic route, low yield, unfavorable large-scale production, and increased production cost, so as to increase the processing capacity, shorten the production cycle, The effect of increasing productivity

Active Publication Date: 2015-01-28
SHANGHAI PHARMA GRP QINGDAO GROWFUL PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology helps improve chemical processes by making it faster and more efficient than traditional methods like batch reactors or continuous flow systems.

Problems solved by technology

This patented technical problem addressed in this patent relates to finding an efficient way to prepare voglibose (viglitazone) that has fewer side effects than existing drugs or other similar medicines currently available on the market today.

Method used

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  • Method and device for continuous preparation of Vildagliptin by tubular reaction
  • Method and device for continuous preparation of Vildagliptin by tubular reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] use figure 1 The device shown produces vildagliptin, and the structural parameters of the main equipment are as follows:

[0034] The pipe length of the tubular reactor 5 is 30m, the length of the preheater is 1.0m, and the volume of the reaction liquid receiving tank is 200L;

[0035] The steps are:

[0036] (1) 3-amino-1-adamantanol, 1-chloroacetyl-2-cyanopyrrolidine is dissolved in a mixed solution in a solvent, mixed with a suspension of alkali and a catalyst, and then preheated by a preheater;

[0037] (2) The preheated mixed solution enters the tubular reactor, the residence time of the material in the tubular reactor is 60min, and then the reaction solution discharged from the tubular reactor is collected and filtered, washed and purified to obtain the product.

[0038] The process parameters are as follows:

[0039] The temperature of the preheater is 70°C, the temperature of the tubular reactor is 70°C, and the flow rate of the material in the pipeline is 0....

Embodiment 2

[0043] use figure 1 The device shown produces vildagliptin, and the structural parameters of the main equipment are as follows:

[0044] The pipe length of the tubular reactor 5 is 100m, the length of the preheater is 1.0m, and the volume of the reaction liquid receiving tank is 200L;

[0045] The steps are:

[0046] (1) 3-amino-1-adamantanol, 1-chloroacetyl-2-cyanopyrrolidine is dissolved in a mixed solution in a solvent, mixed with a suspension of alkali and a catalyst, and then preheated by a preheater;

[0047] (2) The preheated mixed solution enters the tubular reactor, the residence time of the material in the tubular reactor is 100min, and then the reaction solution discharged from the tubular reactor is collected and filtered, washed and purified to obtain the product.

[0048] The process parameters are as follows:

[0049] The temperature of the preheater is 50°C, the temperature of the tubular reactor is 50°C, and the flow rate of the material in the pipeline is ...

Embodiment 3

[0053] use figure 1 The device shown produces vildagliptin, and the structural parameters of the main equipment are as follows:

[0054] The pipe length of the tubular reactor 5 is 80m, the length of the preheater is 1.0m, and the volume of the reaction liquid receiving tank is 200L;

[0055] The steps are:

[0056] (1) 3-amino-1-adamantanol, 1-chloroacetyl-2-cyanopyrrolidine is dissolved in a mixed solution in a solvent, mixed with a suspension of alkali and a catalyst, and then preheated by a preheater;

[0057] (2) The preheated mixed solution enters the tubular reactor, the residence time of the material in the tubular reactor is 150min, and then the reaction solution discharged from the tubular reactor is collected and filtered, washed and purified to obtain the product.

[0058] The process parameters are as follows:

[0059] The temperature of the preheater is 80°C, the temperature of the tubular reactor is 80°C, and the flow rate of the material in the pipeline is 0...

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Abstract

The invention relates to a method and a device for continuous preparation of Vildagliptin by tubular reaction; 3-amino-1-adamantanol and 1-chloracetyl-2-cyano pyrrolidine are dissolved in a mixed solution of solvents, then dissolved with an alkali and a catalyst in a suspension of the solvents, mixed, and preheated by a preheater, the preheated mixed solution enters into a tubular reactor at 20-100 DEG C, the residence time of a material in the tubular reactor is 30min-180min, and the reaction solution discharged from the tubular reactor is collected, filtered washed and purified to obtain the product. The method greatly improves the response speed, shortens the production cycle, increases the amount of processing, and can effectively improve the production capacity. In addition, by controlling the reaction temperature, material movement speed, dosage ratio, catalyst amount and alkali dosage, the formation of by-products disubstituted compounds can be effectively avoided.

Description

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Claims

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Application Information

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Owner SHANGHAI PHARMA GRP QINGDAO GROWFUL PHARMA CO LTD
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