Synthesis method of thionyl diacetic acid

A technology of thiomethylene diacetic acid and a synthetic method, which is applied in the direction of mercaptan preparation, sulfide preparation, electrolysis process, etc., can solve the problems of hydrogen sulfide poisonous gas, environmental pollution, yield decline, etc. Effect of reducing pollution and reducing raw material consumption

Active Publication Date: 2021-01-22
武汉本杰明医药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using this method to synthesize will produce obvious side reactions, which will reduce the yield, and the side reactions will produce toxic hydrogen sulfide gas, which is dangerous to operate and pollutes the environment.

Method used

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  • Synthesis method of thionyl diacetic acid
  • Synthesis method of thionyl diacetic acid
  • Synthesis method of thionyl diacetic acid

Examples

Experimental program
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Effect test

example 1

[0025] Step 1. Dissolve homocystine in hydrochloric acid as catholyte, dilute sulfuric acid as anolyte, the anode material of the electrolytic cell is lead-antimony-tin alloy, the cathode material is lead, and a commercially available BPM type bipolar membrane is used between the two poles separated, at an electrolysis temperature of 40°C, a current density of 0.08A / cm 2 , under the condition that the electrolysis time is 10h, the electroreduction reaction is carried out to obtain homocysteine ​​hydrochloride;

[0026] Step 2. Dissolve the homocysteine ​​hydrochloride and chloroacetic acid in water, heat to 40°C, react for 8 hours, lower the temperature and reduce pressure to recover the solvent water, add methanol to control the temperature at 40°C, and add SO 4 -2 / TiO 2 and thionyl chloride, stirred and reacted for 5h, cooled, filtered out to obtain homoserine lactone hydrochloride, and the filtrate was distilled under reduced pressure to obtain methyl thioglycolate, wher...

example 2

[0029] Step 1, make a film with polystyrene mixed with metal complexes as the intermediate interface catalyst layer, stick the commercially available sulfonic acid type cation exchange membrane, the described intermediate interface catalyst layer, and the commercially available quaternary ammonium salt type anion exchange membrane combined to form a self-made bipolar membrane;

[0030] Step 2, dissolving homocystine in hydrochloric acid as catholyte, dilute sulfuric acid as anolyte, the anode material of the electrolytic cell is lead-antimony-tin alloy, the cathode material is lead, and the two poles are separated by the above-mentioned self-made bipolar membrane , at an electrolysis temperature of 30°C, a current density of 0.09A / cm 2 , under the condition that the electrolysis time is 8 hours, the electroreduction reaction is carried out to obtain homocysteine ​​hydrochloride;

[0031] Step 3: Dissolve the homocysteine ​​hydrochloride and chloroacetic acid in water, heat to...

example 3

[0034] Step 1, using the solution phase inversion method to prepare sulfonic acid type cation exchange membrane and quaternary ammonium salt type anion exchange membrane with finger-like pore structure, dissolve polystyrene particles in organic solvent, add metal complex and mix, use The mixed solution is spun on the surface of the cation-exchange membrane by electrospinning, and then the anion-exchange membrane is glued and fixed on the surface of the cation-exchange membrane spun with polystyrene-metal complex to prepare a self-made bismuth polar membrane.

[0035] Step 2, dissolving homocystine in hydrochloric acid as catholyte, dilute sulfuric acid as anolyte, the anode material of the electrolytic cell is lead-antimony-tin alloy, the cathode material is lead, and the two poles are separated by the above-mentioned self-made bipolar membrane , at an electrolysis temperature of 30°C, a current density of 0.09A / cm 2 , under the condition that the electrolysis time is 8 hours...

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Abstract

The invention discloses a synthesis method of thionyl diacetic acid. The method mainly comprises the following steps: dissolving homocystine in hydrochloric acid to obtain a catholyte, and carrying out an electroreduction reaction in an electrolytic cell to obtain homocysteine hydrochloride; dissolving the homocysteine hydrochloride and chloroacetic acid in water, adding methanol, dropwise addinga catalyst and a dehydrating agent, stirring to react for 2-5 hours, cooling the reaction product, filtering the reaction product to separate out homoserine lactone hydrochloride, and carrying out reduced pressure distillation on the filtrate to obtain methyl mercaptoacetate; and dissolving the methyl mercaptoacetate and the halogenated methyl acetate in methanol, controlling the temperature to be25-50 DEG C, reacting for 6-12 hours, carrying out reduced pressure distillation, adding dilute sulfuric acid, heating the mixture to 50-80 DEG C, and separating and purifying the mixture to obtain the thiodiacetic acid. According to the synthesis method of the thionyl diacetic acid, the yield can be effectively improved.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis. More specifically, the present invention relates to a kind of synthetic method of thiodiacetic acid. Background technique [0002] Thiodiacetic acid is a carboxylic acid organic compound, which can be used as an intermediate in drug synthesis. In the prior art, when synthesizing thiodiacetic acid, sodium chloroacetate and sodium sulfide are commonly used to react to generate sodium thiodiacetic acid, which is then acidified to finally obtain thiodiacetic acid. Synthesis using this method will produce obvious side reactions, which will reduce the yield, and the side reactions will produce toxic hydrogen sulfide gas, which is dangerous to operate and pollutes the environment. Contents of the invention [0003] It is an object of the present invention to solve at least the above-mentioned problems and to provide at least the advantages which will be described later. [0004] Another ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/25C25B3/09C07C319/14C07C323/52
CPCC07C319/12C07C319/14C07C323/52
Inventor 胡林林马婷
Owner 武汉本杰明医药股份有限公司
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