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Method for synthesizing 2-mercaptosuccinic acid

The technology of a kind of mercaptosuccinic acid and its synthesis method is applied in the field of preparation of 2-mercaptosuccinic acid, which can solve problems such as unfavorable industrial large-scale production, inability to separate inorganic salts, unfavorable production costs, etc., and achieve easy industrialization Large-scale production, convenient operation and low cost

Inactive Publication Date: 2011-04-27
YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because acetone is used as a solvent and needs to be heated to reflux when synthesizing the intermediate, its low boiling point will cause a large loss in the long-term reaction process, which is not conducive to controlling production costs
When the hydrolysis reaction is completed, the post-treatment method provided by this patent cannot effectively separate the target product from the generated inorganic salt, so it is not conducive to large-scale industrial production

Method used

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  • Method for synthesizing 2-mercaptosuccinic acid
  • Method for synthesizing 2-mercaptosuccinic acid
  • Method for synthesizing 2-mercaptosuccinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] To a 250 mL three-necked flask equipped with mechanical stirring and a reflux condenser was added 24.6 g of maleic anhydride followed by 130 g of glacial acetic acid. After the solids were dissolved, 19.0 g of thiourea was added with stirring. The reaction system was stirred at room temperature for 12 hours. After filtration, the filter cake was washed twice with glacial acetic acid and water, respectively. After drying, 43.2 g of a white solid was obtained with a yield of 99%.

[0030] The obtained intermediate (III) was added to 120 g of an aqueous solution of 49.6 g of NaOH, and then heated under reflux for reaction for 4 hours. After the reaction system was cooled, it was acidified to pH 3 with 36%-38% concentrated hydrochloric acid. Part of the solvent was evaporated under reduced pressure to about 20 mL of remaining water, heated to reflux at 110° C. for 10 minutes, then cooled, filtered with suction, and washed with a small amount of cold water to obtain a whi...

Embodiment 2

[0034] To a 500 mL three-necked flask equipped with mechanical stirring and a reflux condenser was added 49.1 g of maleic anhydride followed by 250 g of glacial acetic acid. After the solids were dissolved, 38.0 g of thiourea was added with stirring. The reaction system was stirred at room temperature for 12 hours. After filtration, the filter cake was washed twice with glacial acetic acid and water, respectively. After drying, 86.2 g of a white solid was obtained with a yield of 99%.

[0035] The obtained intermediate (III) was added to 200 g of an aqueous solution of 99.0 g of NaOH, and then heated under reflux for reaction for 4 hours. After the reaction system was cooled, it was acidified to pH 3 with 36%-38% concentrated hydrochloric acid. Part of the solvent was evaporated under reduced pressure to about 40 mL of remaining water, continued to heat under reflux for 10 minutes, then cooled, filtered with suction, and washed with a small amount of cold water to obtain a ...

Embodiment 3

[0038] To a 1 L three-necked flask equipped with mechanical stirring and a reflux condenser was added 98.1 g of maleic anhydride followed by 500 g of glacial acetic acid. After the solids were dissolved, 76.0 g of thiourea was added with stirring. The reaction system was stirred at room temperature for 12 hours. After filtration, the filter cake was washed twice with glacial acetic acid and water, respectively. After drying, a white solid 170.6 was obtained in 98% yield.

[0039] The obtained intermediate (III) was added to 400 g of an aqueous solution of 195.9 g of NaOH, and then heated under reflux for reaction for 4 hours. After the reaction system was cooled, it was acidified to pH 3 with 36%-38% concentrated hydrochloric acid. Part of the solvent was evaporated under reduced pressure to about 120 mL of remaining water, heated to reflux for 10 minutes, then cooled, filtered with suction, and washed with a small amount of cold water to obtain a white solid and a pale yel...

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Abstract

The invention discloses a method for synthesizing 2-mercaptosuccinic acid, relates to the technical field of fine chemical engineering, in particular to a method for preparing the 2-mercaptosuccinic acid. The invention provides a method for synthesizing the 2-mercaptosuccinic acid. For fulfilling the aim, the invention has the following technical scheme that: maleic anhydride and thiourea are taken as raw materials, and an intermediate compound, namely 2-amidinothioalkylsuccinic anhydride is synthesized through addition reaction; and under the alkaline condition, the 2-amidinothioalkylsuccinic anhydride is subjected to hydrolysis reaction to generate the 2-mercaptosuccinic acid.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, and more particularly, to a preparation method of 2-mercaptosuccinic acid. Background technique [0002] 2-Mercaptosuccinic acid can be used as complexometric titration masking agent, heavy metal antidote, and can be used in biochemical research and rubber industry. It is also the main component of cold blanching agent and has important application value. At present, 2-mercaptosuccinic acid is usually synthesized by hydrating maleic anhydride to generate maleic acid, and then reacting with hydrogen sulfide to obtain this product. Patent US 6689907B1 adopts this route, but the final total yield of this synthesis method is low, only 75%. Hydrogen sulfide gas is used in the synthesis process of this method, which is not easy to carry out post-treatment and easily causes environmental pollution. In addition, the amount of alkali used in the synthesis process, that is, sodium hydroxide, is al...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/02
Inventor 陈令新王文海王锐
Owner YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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