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Method for purifying compound through ultrasonic crystal precipitation

A technology for compounds and target compounds, applied in chemical instruments and methods, dissolution methods, chemical/physical processes, etc., can solve the problems of low purity, time-consuming and labor-intensive, etc., and achieve improved purity, short time-consuming, detection and determination. convenient effect

Inactive Publication Date: 2015-11-11
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a method for purifying compounds by ultrasonic crystallization. The method for purifying compounds by ultrasonic crystallization solves the problem of passing through columns in the prior art. Purification of organic compounds is time-consuming and labor-intensive, and the technical problem of low purity

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  • Method for purifying compound through ultrasonic crystal precipitation
  • Method for purifying compound through ultrasonic crystal precipitation

Examples

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Embodiment 1

[0021] This example dabigatran etexilate synthetic process intermediate 3-[(3-amino-4-methylaminobenzoyl) (pyridin-2-yl)-amino] the synthesis of ethyl propionate is an example, described The synthetic reaction equation is as follows:

[0022]

[0023] The specific steps of the synthesis of the above reaction and the post-processing method of ultrasonic crystal forcing are as follows:

[0024] (1) Weigh A5.0g into a 250ml round bottom flask, add 10ml water and 10ml acetic acid to dissolve, stir for 2-5 minutes;

[0025] (2) Add 3.0g of zinc powder, stir and react at room temperature for 1 hour;

[0026] (3) After the reaction is completed, suction filtration is performed, and the filtrate is extracted with dichloromethane, and the dichloromethane phase is concentrated to obtain a reddish-brown oily substance B (containing impurities and pigments), with a purity of 87.5%.

[0027] (4) Add about 1-3ml of dichloromethane, force it to just dissolve under ultrasonication, then ...

Embodiment 2

[0031] This example dabigatran etexilate synthetic process intermediate 3-[(3-amino-4-methylaminobenzoyl) (pyridin-2-yl)-amino] synthetic of ethyl propionate, described synthetic reaction The equation is as follows:

[0032]

[0033] The synthetic concrete steps of above-mentioned reaction are as follows:

[0034] (1) Weigh A20g into a 500ml round bottom flask, add 50ml water and 50ml acetic acid to dissolve, stir for 2-5 minutes;

[0035] (2) Add 13g of zinc powder, stir and react at room temperature for 1 hour;

[0036] (3) After the reaction was completed, suction filtered, the filtrate was extracted with dichloromethane, and the dichloromethane phase was concentrated to obtain reddish-brown oil B (containing impurities and pigments), with a purity of 86.7%.

[0037] (4) Add about 3-5ml of dichloromethane, force it to just dissolve under ultrasonication, then add about 5-7ml of ethyl acetate, and continue ultrasonication until solids are precipitated;

[0038] (5) Suc...

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Abstract

The invention relates to a method for purifying a compound through ultrasonic crystal precipitation. According to the method, after completing an organic synthesis reaction, a dissolved amount of a first organic solvent is added to the obtained crude product, and ultrasonic dissolving is performed; a second organic solvent is added after completely dissolving, and ultrasonic dissolving is performed, wherein the addition amount of the second organic solvent is 1-3 times the volume of the first organic solvent; and after the target compound is precipitated from the solution, suction filtration is performed, and washing is performed with a mixed solution of the first organic solvent and the second organic solvent so as to obtain the high-purity target compound. According to the present invention, the ultrasonic crystal precipitation method is used, such that the byproducts and the pigment generated during the organic synthesis reaction can be removed, the purity of the target product during the organic synthesis is substantially increased, and the high-purity target compound is obtained.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a method for purifying compounds, in particular to a post-treatment method for organic synthesis reactions, in particular to a method for purifying compounds by ultrasonic crystallization. Background technique [0002] Organic synthesis reactions play a vital role in the field of organic synthesis and even the entire chemical industry. Improving the process route of organic synthesis and optimizing reaction conditions are the needs of the industry and the driving force for industrial progress. [0003] In the process of organic synthesis, especially in some synthesis with relatively large molecular weight, complex structure and long process route, the synthesis reaction of many compounds is not a simple and complete reaction, and is generally accompanied by the formation of various by-products, even Some pigment is formed. This directly affects the next reaction of the process rout...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/55B01F1/00B01J19/10
CPCB01J19/10C07D213/55B01F21/02
Inventor 任玉杰任卫新
Owner SHANGHAI INST OF TECH
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