- 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
(2019/05/08)
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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; 0042; 0043; 0044; 0045
(2018/11/03)
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