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Preparation method of high-purity D-cystine

A cystine, high-purity technology, applied in the field of high-purity D-cystine synthesis, can solve the problems of D-cysteine ​​L-tartaric acid difficult to completely remove, poor applicability, low optical purity, etc., to achieve easy The effect of production operation, easy control and simple production process

Pending Publication Date: 2021-02-05
山东嘉成医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since this preparation method is easy to make D-2,2'-dimethyltetrahydrothiazole-4-carboxylic acid tartrate entrain L-2,2'-dimethyltetrahydrothiazole-4-carboxylic acid tartrate or L- Cysteine, resulting in low optical purity of the salt, and D-cysteine ​​is easy to oxidize and the entrained L-tartaric acid is difficult to completely remove, the applicability of this method is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation method of embodiment 1 D-cystine, comprises the steps:

[0023] (1) Add 100g of D-2,2-dimethyltetrahydrothiazole-4-carboxylic acid L-tartrate to 8 times the weight of purified water, hydrolyze under reduced pressure at 20°C for 0.5 hours, and then cool down the hydrolyzate to 0°C, adjust pH=4.2-4.5 with potassium carbonate, produce L-potassium hydrogen tartrate precipitate, filter to remove L-potassium hydrogen tartrate, and use the filtrate for later use; after drying, weigh L-potassium hydrogen tartrate, the yield is 98.2 %.

[0024] (2) Oxidation reaction: specifically: the filtrate is adjusted to pH=4.0-5.0 with 5% sodium carbonate aqueous solution and 5% dilute hydrochloric acid, the temperature is controlled at 5°C, and 15g of 12.5% ​​hydrogen peroxide is slowly added dropwise for oxidation. Keep stirring at high temperature for 1 hour, at this time, the pH of the feed liquid is detected to be between 6.5-7.0; filter and wash with water; obtain D-...

Embodiment 2

[0025] The preparation method of embodiment 2 D-cystine, comprises the steps:

[0026] (1) Add 100g of D-2,2-dimethyltetrahydrothiazole-4-carboxylic acid L-tartrate to 15 times the weight of purified water, hydrolyze under reduced pressure at 30°C for 0.5 hours, and then cool down the hydrolyzate to 5°C, adjust the pH to 4.2-4.5 with sodium carbonate, and precipitate L-sodium hydrogen tartrate, filter to remove L-potassium hydrogen tartrate, and use the filtrate for later use; after drying, weigh L-sodium hydrogen tartrate, and the yield is 98 %.

[0027] (2) Oxidation reaction: Specifically: the filtrate is adjusted to pH = 4.2-4.8 with 5% sodium carbonate aqueous solution and 5% dilute hydrochloric acid, the temperature is controlled at 10°C, and 15g of 12.5% ​​hydrogen peroxide is slowly added dropwise for oxidation. Keep stirring at high temperature for 1 hour, at this time, the pH of the feed liquid is detected to be between 6.5-7.0; filter and wash with water; obtain D-...

Embodiment 3

[0028] The preparation method of embodiment 3 D-cystine, comprises the steps:

[0029] (1) Add 100g of D-2,2-dimethyltetrahydrothiazole-4-carboxylic acid L-tartrate to 10 times the weight of purified water, hydrolyze under reduced pressure at 25°C for 0.5 hours, and then cool down the hydrolyzate to 3°C, adjust the pH to 4.2-4.5 with potassium carbonate, and precipitate L-potassium hydrogen tartrate, filter to remove L-potassium hydrogen tartrate, and use the filtrate for later use; after drying, weigh L-potassium hydrogen tartrate, and the yield is 98.5 %.

[0030] (2) Oxidation reaction: specifically: the filtrate is adjusted to pH=4.0-5.0 with 5% sodium carbonate aqueous solution and 5% dilute hydrochloric acid, the temperature is controlled at 8°C, and 15g of 12.5% ​​hydrogen peroxide is slowly added dropwise for oxidation. Keep stirring at high temperature for 1 hour, at this time, the pH of the feed liquid is detected to be between 6.5-7.0; filter and wash with water; o...

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Abstract

The invention discloses a preparation method of high-purity D-cystine. The preparation method comprises the following steps: hydrolyzing D-2, 2-dimethyltetrahydrothiazole-4-carboxylic acid.L-tartrate,and converting the hydrolysate, specifically, converting L-tartaric acid in the hydrolysate into Lentinite, which is separated out as a precipitate; then, before the filtrate is oxidized, the pH value of the filtrate is firstly reduced so that introduction of more impurities in the oxidation process is reduced, and high-purity and high-yield D-cysteine is obtained; the whole preparation method issimple in production process, safe in used raw materials, easy to control, free of high-temperature and high-pressure reaction, low in equipment investment and easy to produce and operate.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing high-purity D-cystine with low production cost, convenient operation and high yield. Background technique [0002] D-cysteine ​​is an important intermediate of the third-generation cephalosporin antibiotic drug-cefomizole sodium. The action properties of cefminox sodium are similar to those of the third-generation cephalosporins, and the finished product is heptahydrate, which has antibacterial effects on E. The production of lipoproteins from peptidoglycan in the bacterial wall is hindered. The lipoprotein structure is unique to Gram-negative bacteria, so its effect on Gram-negative bacteria is stronger than other similar drugs. At the same time, D-cysteine ​​hydrochloride is also a strong inhibitor of Escherichia coli and an effective reliever of acute alcoholism. With the increase in the use of cefminox sodium, the demand for its...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/22C07C319/28C07C319/24C07C323/58
CPCC07C319/22C07C319/28C07C319/24C07B2200/09
Inventor 王平生赵士杰梁志红刘宏林
Owner 山东嘉成医药科技有限公司
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