Method for separating and purifying mercaptosuccinic acid

A technology of thiomalic acid and malic acid, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem that 2-mercaptosuccinic acid cannot be purified and does not directly process 2-mercaptosuccinic acid. Acid reaction solution or crude product, etc., to achieve the effect of strong method applicability, low requirements for operation proficiency and low cost

Inactive Publication Date: 2018-12-28
HENGSHENG TECH R&D CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not realize the purpose of directly processing the 2-mercaptosuccinic acid reaction solution or the crude product. The white solid contains mainly sodium chloride, only a small part of 2-mercaptosuccinic acid, and 2-mercaptosuccinic acid in the light yellow filtrate. cannot be purified

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A method for separating and purifying thiomalic acid:

[0036] (1) The original reaction solution obtained by alkaline hydrolysis to prepare thiomalic acid was evaporated to remove part of the solvent to about 200mL of remaining water, filtered while it was hot, the filtrate was cooled and crystallized, filtered, and dried to obtain 66.7g of crude thiomalic acid, collected Yield 89.2%, purity 88.6%;

[0037] (2) Add 200 mL of 2-pentanone to the obtained crude thiomalic acid, shake and extract in a water-bath shaker at 50°C for 10 h, filter, evaporate the filtrate to remove the solvent, and obtain 65.6 g of thiomalic acid with a purity of 99.5%.

[0038] Wherein, the acquisition of original reaction solution in step (1) is as follows:

[0039] Add 49.0g of maleic anhydride to a 500mL three-necked flask equipped with magnetic stirring and a reflux condenser, and then add 250mL of glacial acetic acid. After the solid dissolves, add 38.1g of thiourea while stirring. The r...

Embodiment 2

[0041] A method for separating and purifying thiomalic acid:

[0042] (1) The original reaction solution obtained by alkaline hydrolysis to prepare thiomalic acid was evaporated to remove part of the solvent to about 50mL of remaining water, filtered while it was hot, the filtrate was cooled and crystallized, filtered, and dried to obtain 13.3g of crude thiomalic acid, collected Yield 88.7%, purity 91.2%;

[0043] (2) Add 15 mL of 3-pentanone to the obtained crude thiomalic acid, shake and extract in a water-bath shaker at 80°C for 1 hour, filter, evaporate the filtrate to remove the solvent, and obtain 13.0 g of thiomalic acid with a purity of 99.4%.

[0044] Wherein, the acquisition of original reaction solution in step (1) is as follows:

[0045] Add 9.8g of maleic anhydride to a 100mL three-necked flask equipped with magnetic stirring and a reflux condenser, and then add 50mL of glacial acetic acid. After the solid dissolves, add 7.6g of thiourea under stirring. The reac...

Embodiment 3

[0047] A method for separating and purifying thiomalic acid:

[0048] (1) The original reaction solution obtained by alkaline hydrolysis to prepare thiomalic acid was evaporated to remove part of the solvent to about 400mL of remaining water, filtered while it was hot, the filtrate was cooled and crystallized, filtered, and dried to obtain 135.9g of crude thiomalic acid, collected Yield 90.6%, purity 80.3%;

[0049] (2) Add 1000mL of 3-methyl-2-pentanone to the obtained crude thiomalic acid, shake and extract in a water-bath shaker at 50°C for 10h, filter, evaporate the filtrate to remove the solvent, and obtain 133.5g of thiomalic acid with a purity of 99.5% .

[0050] Wherein, the acquisition of original reaction solution in step (1) is as follows:

[0051] Add 98.1g of maleic anhydride to a 1000mL three-necked flask equipped with magnetic stirring and a reflux condenser, and then add 500mL of glacial acetic acid. After the solid dissolves, add 76g of thiourea under stirri...

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Abstract

The invention relates to a method for separating and purifying a mercaptosuccinic acid. The method comprises the following steps: taking a raw product of the mercaptosuccinic acid as the raw material,extracting by using an organic extracting agent, filtering, evaporating a solvent in a filtrate to obtain the purified mercaptosuccinic acid; wherein the boiling point of the organic extracting agentis 75-200 DEG C, the relative volatility with n-butyl acetate at the temperature of 25 DEG C is 0.5-4.5, and the organic extracting agent is slightly soluble or insoluble in water. The method efficiently separates the inorganic salt and other byproducts produced in the preparation process, a product of the mercaptosuccinic acid with the purity higher than 99 wt% is obtained, the method not only treats a primary reaction solution obtained in the preparation of the mercaptosuccinic acid through alkali hydrolysis, but also purifies the raw product of the mercaptosuccinic acid obtained in other ways, and the applicability of the method is strong.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for separating and purifying thiomalic acid. Background technique [0002] Thiomalic acid, also known as mercaptosuccinic acid and thiosuccinic acid, is a multifunctional compound and an important chiral intermediate in organic synthesis. It is widely used in various biologically active sulfides such as antibacterial, antituberculosis and antibacterial In the synthesis of leukemia drugs. Thiomalic acid can be used as a complexometric titration masking agent, heavy metal antidote, and can be used in fluorescent probes to detect metal ions. It is a raw material for the preparation of various sulfur-containing drugs, and is also the main component of cold perm agents and additives for cleaning gold plating. It has important application value. [0003] The synthesis of thiomalic acid has been reported mainly aspartic acid method, phosphorothioate method, maleic acid method an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/28C07C323/52
CPCC07C319/28C07C323/52
Inventor 唐海燕张磊张笛徐红彬张懿
Owner HENGSHENG TECH R&D CO LTD
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