Preparation method of L-cystine with high light transmittance

A technology with high light transmittance and cystine, applied in the preparation of organic compounds, chemical instruments and methods, hydrogenated polysulfide/polysulfide preparation, etc., can solve the problems that cannot meet the needs of industrial production, are not suitable for industrial production, reaction Long time and other problems, to avoid the reduction of light transmittance, less side reactions, high selectivity effect

Pending Publication Date: 2022-07-01
SHANXI YUNPENG PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The Chinese patent literature publication number is CN1081917221A, and the patent name is " method for purifying L-cysteine ​​" and comprises the following steps: (1) hydrolysis (2) neutralization (3) decolorization (4) refining, the method prepares L-cysteine The raw material of amino acid is hair extract, which is cheap and easy to obtain, but the disadvantages of this method are: long reaction time, cumbersome post-treatment, many wastes, and low extraction efficiency; therefore, it cannot meet the needs of industrial production
The preparation of this method can obtain L-cysteine ​​with high purity and high yield, but the disadvantages of this method are: the need to use ion exchangers, and the post-treatment of a large amount of hydrochloric acid is cumbersome, and there are many wastes
The disadvantage of this method is that it uses high temperature and high pressure technology and ultrasonic equipment, which requires high equipment, poor safety, and is not suitable for industrial production.

Method used

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  • Preparation method of L-cystine with high light transmittance
  • Preparation method of L-cystine with high light transmittance
  • Preparation method of L-cystine with high light transmittance

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preparation example Construction

[0035] A preparation method of high transmittance L-cystine, the specific steps are as follows:

[0036] S1. add L-cysteine ​​hydrochloride monohydrate into purified water, stir until dissolved, and then adjust pH with inorganic base stirring to obtain solution A;

[0037] S2. add oxidizing agent in the solution A that S1 obtains, react to finish obtaining solution B;

[0038] S3. the solution B obtained by S2 is cooled and stirred for crystallization, filtered to obtain the L-cystine crude product;

[0039] S4. The L-cystine crude product obtained in S3 is washed with purified water, filter cake, and air-dried to obtain the L-cystine finished product.

[0040] The reaction equation is as follows:

[0041]

[0042] Further, the inorganic bases in S1 include but are not limited to one or more of sodium hydroxide, potassium hydroxide, ammonia water, sodium carbonate, and sodium bicarbonate.

[0043] Further, in the S1, adjust the pH to 7-8 to stop stirring.

[0044] Furth...

Embodiment 1

[0052] Add 50g cysteine ​​hydrochloride monohydrate and 250g purified water to a 500ml brown four-necked bottle, stir until all dissolved, cool to 5°C, add ammonia water dropwise to adjust pH=8.1, stop stirring, and keep the temperature at 5- 10°C, dropwise add 72.8g of 20% hydrogen peroxide, naturally heat up to room temperature, keep the temperature for 4h, cool to 5-10°C for crystallization for 2h, from the start of the reaction to the end of crystallization, stir every 2h, filter, 20g purified water The filter cake was washed and dried to constant weight at 55-65°C to obtain 32.5 g of L-cystine crude product.

Embodiment 2

[0054]Add 50g of cysteine ​​hydrochloride monohydrate and 300g of purified water to a 500ml brown four-necked flask, stir until all dissolved, cool to 5°C, dropwise add 5% sodium hydroxide solution to adjust pH=7.5, stop stirring, Keep the temperature at 5-10°C, add 25.13g of DMSO dropwise, heat up to room temperature naturally, keep the reaction for 4h, the reaction is over, cool down to 5-10°C for crystallization for 3h, from the start of the reaction to the end of the crystallization, stir every 2h, Filter, wash the filter cake with 20 g of purified water, and dry to constant weight at 55-65 °C to obtain 31.77 g of crude cystine.

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Abstract

The invention relates to the technical field of pharmaceutical chemical preparation, in particular to a preparation method of high-light-transmittance L-cystine. The preparation method comprises the following specific steps: adding L-cysteine hydrochloride monohydrate into purified water, stirring until the L-cysteine hydrochloride monohydrate is dissolved, and stirring with inorganic alkali to adjust the pH value, so as to obtain a solution A; adding an oxidizing agent into the solution A, and reacting to obtain a solution B; cooling, stirring and crystallizing the solution B, and filtering to obtain an L-cystine crude product; and washing the L-cystine crude product with purified water, and carrying out forced air drying on a filter cake to obtain an L-cystine finished product. The reaction and crystallization are carried out in a standing state, large-crystal cystine is easily and stably prepared, and the problem that the light transmittance of cystine is reduced due to the fact that the crystal is fine and is not easy to dissolve in hydrochloric acid and the fine crystal is easy to adsorb impurities is effectively avoided. No catalyst is used, high-temperature and high-pressure reaction is avoided, reaction conditions are mild, required equipment is simple, and the method is suitable for large-scale industrial production. The method has the advantages of cheap and easily available raw materials, simple operation and few three wastes.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical chemical preparation, and more particularly, to a preparation method of L-cystine with high light transmittance. Background technique [0002] L-cystine has chemical name: L-3,3'-dithiobis(2-aminopropionic acid), molecular formula: C 6 H 12 N 2 O 4 S 2, Molecular weight: 240.30, white flaky crystal or crystalline powder, very slightly soluble in water, insoluble in ethanol and other organic solvents, easily soluble in dilute acid and alkaline solution, easily decomposed in hot alkaline solution [0003] Structural formula: [0004] [0005] L-cystine was discovered in 1810 by Wollaston from bladder stones. In 1832, Berzelius named it cystine, which is a sulfur-containing amino acid, which exists in a small amount in protein and is mostly contained in keratin such as hair, fingers and claws, and can also be obtained by synthetic methods. As an important pharmaceutical intermediate,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/24C07C319/28C07C323/58
CPCC07C319/24C07C319/28C07B2200/07C07C323/58
Inventor 刘向男
Owner SHANXI YUNPENG PHARMA
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