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The synthetic method of dl-homocysteine ​​thiolactone hydrochloride

A technique for synthesizing cystine thiolactone and its method, which is applied in the field of synthesis of DL-homocysteine ​​thiolactone hydrochloride, can solve problems such as operational hazards, a large amount of hydrogen waste water, and pollute the environment, and achieve an increase in production efficiency, high cathode activity, and improved mechanical strength

Active Publication Date: 2019-12-31
武汉本杰明医药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the prior art, metal zinc or tin and hydrochloric acid are commonly used to carry out reduction reaction with DL-homocystine when synthesizing the drug. Using this synthesis method will produce a large amount of hydrogen, zinc salt (tin salt) and a large amount of waste water, which is very polluting environment, and the operation is very dangerous

Method used

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  • The synthetic method of dl-homocysteine ​​thiolactone hydrochloride
  • The synthetic method of dl-homocysteine ​​thiolactone hydrochloride
  • The synthetic method of dl-homocysteine ​​thiolactone hydrochloride

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Embodiment 1

[0025] Preparation of the cathode electrode in the electrolytic cell: the entire surface of the glassy carbon electrode is roughened to a roughness of 10 microns to obtain a substrate, and the surface roughness is measured by a stylus-type roughness meter, and the average is calculated using the JIS B0601:2001 standard roughness. Grind the lead-bismuth alloy powder and place it in a CVD furnace, pass argon gas at a rate of 5 sccm, place the substrate downstream of the argon gas, raise the temperature to 650 °C at a heating rate of 25 °C / min, keep it warm for 1 hour, and then cool it down. A lead-bismuth alloy thin film is formed on the base material to obtain a cathode electrode, a titanium plate is used as an anode, and the cathode electrode and the anode electrode are applied to an ion diaphragm electrolytic cell.

[0026] 200kg DL-homocystine is completely dissolved in a hydrochloric acid solution with a mass fraction of 8%, and a total of about 373L of catholyte is used. T...

Embodiment 2

[0030] Add 300kg DL-methionine, 750kg concentrated sulfuric acid with a mass fraction of 98%, and 90kg nickel-based metal-supported catalyst to the autoclave, pressurize to 2Mpa, control the temperature at 120°C, and react for 7 hours to obtain a hydrolyzate; The solution was adjusted to pH 5 with 30% sodium hydroxide solution, decolorized with 4kg of activated carbon, filtered after decolorization, concentrated and crystallized the filtrate, rinsed twice with alcohol, and dried to obtain 196.1kg of DL-homocystine Acid, the product yield of DL-homocysteine ​​is 72.7% (based on DL-methionine), and its purity is 99.9%.

[0031] Preparation of the cathode electrode in the electrolytic cell: the entire surface of the glassy carbon electrode is roughened to a roughness of 10 microns to obtain a substrate, and the surface roughness is measured by a stylus-type roughness meter, and the average is calculated using the JIS B0601:2001 standard roughness. Grind the lead-bismuth alloy po...

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Abstract

The invention discloses a synthesis method of DL-homocysteine thiolactone hydrochloride. A DL-homocystine is prepared into a catholyte with a hydrochloric acid solution as a medium, and electrolysis is conducted in an electrolysis tank to obtain the DL-homocysteine thiolactone hydrochloride, wherein according to a cathode electrode, a roughened glass carbon electrode serves as a base material, andthe surface of the base material is covered with lead-bismuth alloy. The method can be used for improving the yield of the DL-homocysteine thiolactone hydrochloride.

Description

technical field [0001] The present invention relates to the field of compound synthesis. More specifically, the present invention relates to a synthetic method of DL-homocysteine ​​thiolactone hydrochloride. Background technique [0002] DL-homocysteine ​​thiolactone hydrochloride is a biochemical reagent and pharmaceutical intermediate, which can be used to prepare citivolone, erdosteine ​​and other drugs. In the prior art, metal zinc or tin and hydrochloric acid are commonly used to carry out reduction reaction with DL-homocystine when synthesizing the drug. Using this synthesis method will produce a large amount of hydrogen, zinc salt (tin salt) and a large amount of waste water, which is very polluting environment, and the operation is very dangerous. Contents of the invention [0003] The purpose of the present invention is to provide a synthetic method for DL-homocysteine ​​thiolactone hydrochloride to improve the synthetic yield. [0004] In order to realize thes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/00C25B11/12C07D333/32
Inventor 胡可雄胡林林
Owner 武汉本杰明医药股份有限公司
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