A kind of method for preparing 2,3-sodium dimercaptopropanesulfonate

Abstract

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.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a method for preparing sodium 2,3-dimercaptopropanesulfonate. Background technique [0002] Sodium 2,3-dimercaptopropanesulfonate (Na-DMPS) is currently a more effective detoxification drug for heavy metals such as mercury, arsenic, copper, and cadmium. Its structural formula is as follows: [0003] [0004] The current industrial synthesis process of sodium 2,3-dimercaptopropanesulfonate is derived from the following patents and documents: [0005] 1. U.S. Patent US4382040, using allyl bromide as the starting material, adding allyl sulfonate sodium in water, adding 29% aqueous sodium sulfide solution saturated with hydrogen sulfide to the bromination reaction solution, and reacting at room temperature 16h, deleading with hydrogen sulfide. The literature reports that the total yield reaches 30.6%, and the purity of the finished product reaches 99% (iod...

AI Technical Summary

Problems solved by technology

[0007] 3. Wang Chunyu (CN1432566A), the main reaction conditions are basically the same as the former, the main difference is that the reaction time is shortened by half (10h), the original document did not disclose the yield and purity level

[0012] The above-mentioned sulfhydrylating agents used are all sodium hydrosulfide (potassium). After the sulfhydrylating reaction, the pH is adjusted to 4-5 with acetic acid. During this period, a large amount of highly toxic gas hydrogen sulfide will be produced, and the deleading reaction uses Hydrogen sulfide gas, causing serious environmental pollution

Moreover, some patents use pressurized conditions, and industrial production has strict requirements on equipment. There are also patents that use zinc acetate instead of lead acetate to purify sodium dimercaptopropanesulfonate. The product is precipitated, which will inevitably lead to a large amount of inorganic salt in the product, so it has carried out multiple crystallization and purification of the zinc salt, the entire operation process is relatively cumbersome, and the production cycle is long

Images