Preparation of homocystine

A technology of homocystine and methionine, applied in hydrogenated polysulfide/polysulfide preparation, organic chemistry, etc., can solve a large amount of solid waste wastewater, environmental hazards, etc.

Active Publication Date: 2009-01-21
九江中星医药化工有限公司
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  • Abstract
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Problems solved by technology

[0009] The co-heating of methionine and sulfuric acid or the mixed acid of sulfuric acid and hydrohalic acid to prepare homocystine is the only method that can be produced industrially at present, but this method will produce a large amount of solid waste and waste water with high salt content, which will cause serious damage to the environment. harm

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  • Preparation of homocystine
  • Preparation of homocystine
  • Preparation of homocystine

Examples

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Effect test

Embodiment 1

[0063] Heat 40g DL-methionine and 120ml 9mol / L sulfuric acid solution at 125-135°C for 6 hours, cool to room temperature, add 100ml water to dilute to reduce viscosity, and obtain about 200ml reaction solution with sulfuric acid concentration of 4.5mol / L , this reaction solution enters as figure 1 In the stock solution chamber of the diffusion dialysis device shown, 300ml of pure water enters the recovery chamber of the diffusion dialysis device. After 24 hours of diffusion dialysis, the recovery chamber obtains 250ml of sulfuric acid with a sulfuric acid concentration of 1.08mol / L, and the recovery rate of sulfuric acid is about 30%. . The reaction solution obtained in the stock solution chamber is 250ml, and the concentration of sulfuric acid is about 2.5mol / L. After the solution obtained in the stock solution chamber is adsorbed and decolorized by activated carbon, it is neutralized with 30% sodium hydroxide solution until the pH value is about 7, and a total of 125ml of 3...

Embodiment 2

[0065] Heat 40g DL-methionine and 120ml 14mol / L sulfuric acid solution at 105-115°C for 3 hours, cool to room temperature, add 100ml water to dilute to reduce viscosity, and obtain about 200ml reaction solution with sulfuric acid concentration of 7.5mol / L , this reaction solution enters as figure 2 In the dilute chamber of the electrodialysis device shown, 250ml of sulfuric acid solution with a concentration of about 0.3mol / L enters the concentrated chamber, and the liquid in the electrode chamber is 1mol / L sulfuric acid solution. 2 The electric current density electrodialysis 48 hours, reclaims the sulfuric acid that 340ml concentration is 3.56mol / L in the concentration room, and the sulfuric acid recovery rate is about 75%, and average current efficiency is 52.4%. After the solution in the light chamber is adsorbed and decolorized by activated carbon, it is neutralized to about pH 7 with 30% sodium hydroxide solution, and a total of 75 ml of 30% sodium hydroxide solution is...

Embodiment 3

[0067] Heat 40g DL-methionine and 120ml 6mol / L sulfuric acid solution at 135-145°C for 18 hours, cool to room temperature, add 100ml water to dilute to reduce viscosity, and obtain about 200ml reaction solution with sulfuric acid concentration of 2.7mol / L , this reaction solution enters as image 3 In the dilute chamber of the electrodialysis device shown, 250 ml of sulfuric acid solution with a concentration of about 0.3 mol / L enters the concentrated chamber, the anolyte is 1 mol / L sulfuric acid solution, and the catholyte is 1 mol / L sodium hydroxide solution. , at 2A / dm 2 Electrodialysis at a high current density for 65 hours until the pH of the solution in the dilute chamber is about 7. 320ml of sulfuric acid with a concentration of 1.82mol / L was recovered in the concentrated chamber, the recovery rate of sulfuric acid was about 92%, and the average current efficiency was 34.7%. A large amount of solid homocystine has precipitated out of the solution in the light chamber....

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Abstract

A method for preparing homocystine is disclosed. The method capable of eliminating a great amount of pollutants, recycling useful materials, and reducing preparation cost comprises following steps that: methionine together with a 5 to 18mol / L sulfuric acid and a 0 to 50 percent (by weight) halogen acid is heated to and kept at a temperature of 100 to 150 DEG C for 0.5 to 20 hours, with the molar ratio of methionine to sulphuric acid to halogen acid being 1 to 2-6.5 to 0-4; after the reaction liquid is cooled down, the sulfuric acid in the reaction liquid is reclaimed through dialysis until the isoelectric point of homocystine is reached, and then the precipitate is filtrated, washed, and dried to obtain homocystine. The invention is suitable for the preparation of homocystine.

Description

technical field [0001] The invention relates to a method for preparing amino acid containing disulfide bonds, in particular to a method for preparing homocystine. Background technique [0002] Homocysteine ​​is a disulfide-bonded amino acid whose structural formula is: [0003] [0004] The product of reductive cyclization of homocysteine ​​is homocysteine ​​thiolactate, which is a key intermediate for the synthesis of Erdosteine, and the oxidation product of homocysteine ​​is homosulfoalanine, which is a Important pharmaceutical intermediates. [0005] Regarding the synthesis of homocysteine, it was first proposed by Butz and du Vigneaud (J. Biol. Chem., 1932-33, 99, 135) to co-heat methionine with a large amount of excess sulfuric acid, and it is still used today. However, this is not an ideal method because the theoretical yield of homocystine is also only 50%, which is due to the production of a large amount of by-product dimethylsulfonium salt (S-methylmethionine s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/58C07C319/24
Inventor 莫一平张晓忠韦卫东
Owner 九江中星医药化工有限公司
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