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An improved mercaptolation method for the synthesis of sodium 2,3-dimercaptopropanesulfonate

A technology of sodium dimercaptopropanesulfonate and sulfhydrylation, which is applied in the directions of organic chemistry, thiol preparation, etc., can solve the problems of low sulfhydrylation reaction yield, etc., and achieve the effect of high selectivity and high reaction rate

Active Publication Date: 2016-05-25
合肥诚志生物制药有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0012] It can be seen that the existing technical solutions all have the problem of low yield of thiolation reaction, therefore, there is an urgent need for an economical and applicable new process for thiolation reaction

Method used

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  • An improved mercaptolation method for the synthesis of sodium 2,3-dimercaptopropanesulfonate
  • An improved mercaptolation method for the synthesis of sodium 2,3-dimercaptopropanesulfonate
  • An improved mercaptolation method for the synthesis of sodium 2,3-dimercaptopropanesulfonate

Examples

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Embodiment 1

[0034] Embodiment 1 (embodiment of the present invention)

[0035] 1. Preparation of sodium hydrosulfide: 3250ml of absolute ethanol was put into a 5L autoclave, and 110g (1.60mol) of sodium ethoxide was added under stirring. After adding, close and tighten the feeding port, control the internal temperature below 25°C through the jacket cooling water, and feed high-pressure hydrogen sulfide gas into the kettle through the hydrogen sulfide gas cylinder under stirring conditions, and control the pressure within the range of 0.3-0.5MPa Stir the reaction for about 30 minutes, so that the pH value of the solution reaches the range of 6.5-7.5.

[0036] 2. Mercaptolation reaction: After the above reaction is completed, the pressure in the kettle is released, the lid of the kettle is opened, and 230.3g (0.75mol) of sodium 2,3-dibromopropanesulfonate is added at a time. After the addition is complete, tighten the lid of the kettle, and control the internal temperature at 23°C to 25°C...

Embodiment 2（50

[0047] Example 2 (Example of mercaptolation reaction at 50°C)

[0048] In this example, except that the thiolation reaction temperature was changed from room temperature for 90 minutes to 50° C. for 30 minutes, other steps and conditions were exactly the same as those in Example 1 to obtain 260.2 g of lead salt.

[0049] Lead salt content (measured value): 62.02%;

[0050] Lead salt yield: 69.47%.

Embodiment 3

[0051] Embodiment 3 (the pressure control embodiment A of embodiment 1)

[0052] In this example, the other steps and conditions are exactly the same as in Example 1, except that the hydrogen sulfide gas pressure is changed from pressurized to normal pressure during the preparation process of sodium hydrosulfide and the mercaptolation reaction. 191.74 g of lead salt complex was obtained.

[0053] Lead content (measured value): 60.06%;

[0054] Lead salt yield: 49.6%.

[0055] Remarks: when changing the pressurized hydrogen sulfide feeding condition of embodiment 1 into normal pressure feeding, the lead salt quality and yield will obviously decrease.

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Abstract

The invention discloses a novel method for sulfhydrylation reaction in a synthesis process of 2,3-sodium dimercaptosulphonate. Different from the existing sulfhydrylation reaction, the sulfhydrylation reaction is fulfilled by introducing high pressure hydrogen sulfide gas into absolute ethyl alcohol solution of sodium alcoholate to obtain sodium hydrosulfide and then adding 2,3-dibromo-1-propanesulfonic acid sodium salt, and carrying out sulfhydrylation reaction under the condition of continuously introducing high pressure hydrogen sulfide in short time and under the high yield. Therefore, the bottleneck technology of the sulfhydrylation reaction in the synthesis process of 2,3-sodium dimercaptosulphonate, which is very troubled, is successfully solved.

Description

technical field [0001] The invention relates to the improvement of the mercaptolation method in the synthesis process of sodium 2,3-dimercaptopropanesulfonate and its derivatives, and belongs to the field of organic or pharmaceutical synthesis. Background technique [0002] Sodium 2,3-dimeicaptopropane-1-sulfonate (sodium2,3-dimeicaptopropane-1-sulfonate, Na-DMPS) is a metal ion complexing agent containing a mercapto group. As an excellent antidote, it has been widely used in Treatment of acute and chronic poisoning of heavy metals such as mercury, arsenic, copper, lead and cadmium. It is also an important intermediate in dye chemical industry. With the deepening of Na-DMPS application research, more new uses are gradually being discovered. Therefore, it is particularly necessary to further research and improve its preparation process. [0003] Its structural formula is as follows: . [0004] The current industrial synthesis process of Na-DMPS originates from US patent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/66C07C319/02
Inventor 季俊虬高美华李孝常陈军
Owner 合肥诚志生物制药有限公司
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