Synthesis method of DL-homocysteine thiolactone hydrochloride

A technology for the synthesis of cystine thiolactone and its synthesis method, which is applied in the field of synthesis of DL-homocysteine ​​thiolactone hydrochloride, which can solve the problems of polluted environment, dangerous operation, large amounts of hydrogen waste water, etc., and achieve cathode activity High, improve productivity, improve the effect of mechanical strength

Active Publication Date: 2019-06-28
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 synthes...

Method used

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  • Synthesis method of DL-homocysteine thiolactone hydrochloride
  • Synthesis method of DL-homocysteine thiolactone hydrochloride
  • Synthesis method of DL-homocysteine thiolactone hydrochloride

Examples

Experimental program
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Effect test

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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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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