- Method for preparing sodium 2,3-dimercapto-1-propanesulfonate
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The invention belongs to the technical field of drug synthesis, and in particular relates to a method for preparing sodium 2,3-dimercapto-1-propanesulfonate. With sodium allysulfonate used as a starting material and through a bromination reaction, a sulfhydrylation reaction, a lead salt reaction and a lead removal reaction, high-content sodium 2,3-dimercapto-1-propanesulfonate is obtained by refinement. The total yield is 23.2% and above; especially when zinc dust reduction step is added after hydrolysis, the yield can be greatly increased, the total yield can reach 35-41.5%, and the refined sodium 2,3-dimercapto-1-propanesulfonate content reaches 99% and above. Ethanethioic acid potassium salt is used as a sulphurizing agent and then is hydrolyzed under strong acid conditions, and dilutesulfuric acid is used for lead removal after lead formation. During the whole reaction and treatment process, toxic gas hydrogen sulfide which affects the environment is prevented from being used or generated. Thereby, working conditions are improved, emission of three wastes is reduced, and production efficiency is enhanced.
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Paragraph 0038; 0039; 0040; 0047; 0048; 0052; 0053
(2019/05/08)
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- Sodium dimercaptopropansulfonate preparation method
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The invention relates to the field of chemical pharmacy, and specifically provides a sodium dimercaptopropansulfonate preparation method. The sodium dimercaptopropansulfonate preparation method comprises that 1) sodium allyl sulfonate and bromine are subjected to a reaction under the effect of an auxiliary agent to obtain sodium dibromo propansulfonate, wherein the auxiliary agent is selected from sodium bromide, sodium iodide, or a combination thereof; 2) the sodium dibromo propanesulfonate obtained in step 1), sodium hydrosulfide and zinc acetate are subjected to a reaction to obtain a sodium dimercaptopropansulfonate-zinc complex; and 3) the sodium dimercaptopropansulfonate-zinc complex obtained in the step 2) reacts with hydrogen sulfide to obtain the sodium dimercaptopropansulfonate. According to the present invention, the preparation method has characteristics of low toxicity of the used reagent, low environmental pollution, low cost of zinc acetate, low consumption, low cost, simple process, no requirement of high pressure equipment and safe operation, and is suitable for industrial production, and the obtained sodium dimercaptopropansulfonate has the high purity and meets the quality requirements of the bulk drug.
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Paragraph 0069; 0070; 0102-0111
(2017/10/27)
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- A kind of improved 2, 3 - dimercapto method for the synthesis of the sodium
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The invention belongs to the organic or drug synthesis field and relates to a synthetic method of improved sodium 2,3-dimercaptosulphonate. The adopted technical scheme is as follows: sulfhydrylation reaction is adopted, wherein the PH value of sodium (potassium) bisulfide solution is an important process parameter of the sulfhydrylation reaction. Commercial NaHS solids are dissolved with water, halogenated acids such as concentrated hydrochloric acid and the like are used for neutralizing until the PH value is 6.5-7, and then the NaHS solution is reacted with 2,3-dibromo-1-propanesulfonic acid sodium salt; and besides, high-selectivity environment and condition are provided for the sulfhydrylation reaction of sodium 2,3-dimercaptosulphonate, hydrogen sulfide gas which is highly toxic is not used, and the working condition is improved; and furthermore, hydrogen chloride methanol solution is used for deleading reaction, the hydrogen sulfide gas which is highly toxic and has influence on environment is avoided, and the working condition is improved.
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Paragraph 0032; 0035; 0038; 0039
(2018/11/03)
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- An improved synthesis of 2,3-dithiopurine propyl sodium Hydrosulfuryl reaction method
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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.
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Paragraph 0034; 0036; 0092; 0095; 0097; 0102; 0104
(2018/07/10)
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