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A kind of dimercaptosuccinic acid and its salt and preparation method

A technology of dimercaptosuccinate and dimercaptosuccinic acid, which is applied in the field of dimercaptosuccinic acid and its salts and preparation, can solve the problems of high energy consumption, low actual yield, low production capacity, etc., and achieve the preparation method The effect of simple process, short preparation cycle and high purity

Active Publication Date: 2019-06-25
HEFEI LIFEON PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the addition reaction cycle is long, the actual yield is low, and the freeze-drying method needs to be used to remove water after the reaction, so the energy consumption is high, the production capacity is low, and the industrial production value is lacking.
[0012] 2,3-dimercaptobutyrate (such as disodium 2,3-dimercaptobutyrate) can be prepared into water injection for patients with acute heavy metal poisoning. There is no information about 2,3-dimercaptobutyrate in the related art Public Journal Reports of Preparation Methods
In fact, 2,3-dimercaptobutyric acid is used to prepare 2,3-dimercaptobutyric acid salt, because it is difficult to fully convert 2,3-dimercaptobutyric acid into disodium salt, there will be a small amount of dimercaptosuccinic acid crystals and alkali and other impurities, it is difficult to obtain high-purity 2,3-dimercaptobutyrate products

Method used

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  • A kind of dimercaptosuccinic acid and its salt and preparation method
  • A kind of dimercaptosuccinic acid and its salt and preparation method
  • A kind of dimercaptosuccinic acid and its salt and preparation method

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preparation example Construction

[0073] The preparation method of dimercaptosuccinic acid of the present invention is simple in process, and uses a kind of solid ethyl xanthate (sodium salt or potassium salt) with slight odor and low price to replace liquid thioacetic acid with strong odor and unstable quality , and compared with the existing process, one step of elimination reaction is omitted, especially the unsafe addition reaction operation is completely eliminated, which is very beneficial to the future industrial production, the preparation cycle is short, the yield is high, and the cost is low, which is suitable for the promotion of industrial production.

[0074] In a preferred specific embodiment of the present invention, said ethyl xanthate includes one or more of ethyl xanthate metal salts, preferably includes one or more of ethyl xanthate alkali metal salts Various, more preferably sodium ethyl xanthate and / or potassium ethyl xanthate.

[0075] In a preferred embodiment of the present invention, t...

Embodiment 1

[0133] A preparation method for dimercaptosuccinic acid, comprising the steps of:

[0134] 1. Substitution reaction:

[0135] Put 600mL of acetone-water mixed solvent (where the volume ratio of acetone and water is 1:0.8) and 153.1g (content 95.0%, 1.2moL) of potassium ethyl xanthate into a dry and clean 1000mL reaction flask, stir and use The temperature of the water bath was raised to 40-45°C, and 141 g (0.5 moL) of 2,3-dibromosuccinic acid was slowly added after the solution was completely dissolved. After the addition was completed, the temperature was slowly raised to 55° C., and the reaction was continued for 3.0 h, and the end point was determined by HPLC. After the reaction, the reaction solution was slowly cooled to below 15°C, and allowed to stand for 2 hours to allow the precipitation of potassium bromide to fully separate out, and then filtered to remove it. Then the filtrate was vacuum concentrated to 1 / 3 of the original volume and placed in a closed container f...

Embodiment 2

[0147] Under the process of Example 1, the volume ratio of acetone and water in the acetone-water mixed solvent is 1:0.1; the amount of 2,3-dibromosuccinic acid is 169.2g (0.6mol); the substitution reaction is heated to 45 ℃, reacted for 6h; the dilute hydrochloric acid with the mass fraction of 10.0% replaced the aqueous sodium hydroxide solution with the mass fraction of 15.0% in Example 1 as the hydrolysis reaction (nitrogen protection) reagent, and the hydrolysis reaction was heated up to 75 ° C, and the reaction was 6h; acidification temperature Keep at 0°C; other processes and conditions are exactly the same as in Example 1. Finally, 57.7 g of a product of 2,3-dimercaptosuccinic acid was obtained, with a melting point of 191.5°C-192.9°C and a content of 99.60% (HPLC).

[0148] Elemental Analysis Results:

[0149]

[0150] After concentration, decolorization and crystallization from the primary refined mother liquor, 1.98 g of the secondary product was obtained, melti...

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Abstract

The invention relates to the technical field of organic synthesis, in particular to dimercaptosuccinic acid and salt thereof and a preparation method. The preparation method comprises the following steps: carrying out reaction on ethyl xanthate and 2,3-dibromosuccinic acid, so that 2,3-diethyl xanthate-1,4 succinic acid is obtained; hydrolyzing the 2,3-diethyl xanthate-1,4 succinic acid, so that 2,3-dimercaptosuccinate solution is obtained; and acidifying the obtained 2,3-dimercaptosuccinate solution, so that 2,3-dimercaptosuccinic acid is obtained. The preparation method provided by the invention has the advantages that technology is simple, liquid-state thioacetic acid with strong odor and unstable quality does not need to be used, unsafe addition reaction does not need to be carried out, preparation period is short, yield is high, cost is low, and the dimercaptosuccinic acid can be applicable to industrial production and popularization and can be further prepared into a dimercaptosuccinate product. The dimercaptosuccinic acid product and the dimercaptosuccinate product are high in purity and low in cost.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a dimercaptosuccinic acid and its salt and a preparation method. Background technique [0002] Dimercaptosuccinic acid (DMSA) is an excellent heavy metal antidote, its structure is as follows: [0003] [0004] With the continuous deepening of applied research, its application field has expanded to many aspects of industry and daily life. Therefore, in-depth research and improvement of its synthesis process is particularly necessary. [0005] At present, the mainstream industrial synthesis route of DMSA in China is to use 2,3-dibromosuccinic acid as the starting material, which undergoes elimination reaction with caustic alkali to produce the intermediate disodium butynedioate. It undergoes an addition reaction with thioacetic acid under strong acidic conditions to generate 2,3-diacetylthiosuccinic acid. This material does not need to be separated, and it can be h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/12C07C323/52
Inventor 李孝常范冰冰季永明李冰孟宪科
Owner HEFEI LIFEON PHARMA
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