Preparation method of S-carboxymethyl-L-cysteine

A technology of cysteine ​​and carboxymethyl, which is applied in the field of amino acid preparation, can solve the problems of large specific surface area of ​​crystals, easy adsorption of solution impurities, difficult purification process, etc., and achieve the effect of improving purity

Inactive Publication Date: 2020-05-12
NINGBO YUANFA BIOENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the crystals formed by the above method generally have smaller particles, and the particle diameters observed under a microscope are all less than 10um, so that the specific surface area of ​​the crystals is large, and it is easy to absorb impurities in the solution, especially the high content of chlorine, so This makes the subsequent purification process more difficult

Method used

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  • Preparation method of S-carboxymethyl-L-cysteine
  • Preparation method of S-carboxymethyl-L-cysteine

Examples

Experimental program
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Embodiment 1

[0039] A preparation method of S-carboxymethyl-L-cysteine, characterized in that: comprising the following steps,

[0040] Step 1. Dissolve 1mol of L-cysteine ​​hydrochloride monohydrate in 450mL of distilled water, place in ice brine to cool down to 0-5°C, and adjust the pH to 9-10 with 20% sodium hydroxide solution , to obtain solution (a);

[0041] Step 2: Add 1.2 mol of chloroacetic acid into 400 ml of distilled water, stir to dissolve, adjust the pH to 6-7 with 20% sodium hydroxide solution, and obtain solution (b);

[0042] Step 3. Under the protection of nitrogen, drop the solution (b) into the solution (a), and control the temperature in the ice-salt water to 0-5°C. After the dropping, the solution (c) is obtained;

[0043] Step 4: Use 20% sodium hydroxide solution to adjust the pH of the solution (c) to 8, then heat up to 55-60°C, and keep it warm for 1 hour;

[0044] Step 5, the solution (c) is lowered to room temperature, and the pH of the solution (c) is adjusted...

Embodiment 2

[0050] A preparation method of S-carboxymethyl-L-cysteine, characterized in that: comprising the following steps,

[0051] Step 1. Dissolve 1mol of L-cysteine ​​hydrochloride monohydrate in 450mL of distilled water, place in ice brine to cool down to 0-5°C, and adjust the pH to 9-10 with 20% sodium hydroxide solution , to obtain solution (a);

[0052] Step 2: Add 1.3mol of chloroacetic acid into 400ml of distilled water, stir to dissolve, adjust the pH to 6-7 with 20% sodium hydroxide solution, and obtain solution (b);

[0053] Step 3. Under the protection of nitrogen, drop the solution (b) into the solution (a), and control the temperature in the ice-salt water to 0-5°C. After the dropping, the solution (c) is obtained;

[0054]Step 4: Use 20% sodium hydroxide solution to adjust the pH of the solution (c) to 8, then heat up to 55-60°C, and keep it warm for 1 hour;

[0055] Step 5, the solution (c) is lowered to room temperature, and the pH of the solution (c) is adjusted to...

Embodiment 3

[0061] A preparation method of S-carboxymethyl-L-cysteine, characterized in that: comprising the following steps,

[0062] Step 1. Dissolve 1mol of L-cysteine ​​hydrochloride monohydrate in 450mL of distilled water, place in ice brine to cool down to 0-5°C, and adjust the pH to 9-10 with 20% sodium hydroxide solution , to obtain solution (a);

[0063] Step 2: Add 1.4mol of chloroacetic acid into 400ml of distilled water, stir to dissolve, adjust the pH to 6-7 with 20% sodium hydroxide solution, and obtain solution (b);

[0064] Step 3. Under the protection of nitrogen, drop the solution (b) into the solution (a), and control the temperature in the ice-salt water to 0-5°C. After the dropping, the solution (c) is obtained;

[0065] Step 4: Use 20% sodium hydroxide solution to adjust the pH of the solution (c) to 8, then heat up to 55-60°C, and keep it warm for 1 hour;

[0066] Step 5, the solution (c) is lowered to room temperature, and the pH of the solution (c) is adjusted t...

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Abstract

The invention discloses a preparation method of S-carboxymethyl-L-cysteine, which relates to the field of amino acid production, and mainly comprises the following steps: 1, dissolving L-cysteine hydrochloride monohydrate, cooling the solution to 0-5 DEG C, and regulating the pH value to 9-10 to obtain a solution (a); 2, dissolving chloroacetic acid, and adjusting the pH value to 6-7 to obtain a solution (b); 3, dropwise adding the solution (b) into the solution (a), and carrying out heat preservation to obtain a solution (c); 4, adjusting the pH value of the solution (c) to 8, and heating thesolution to react for 1 hour; 5, cooling the solution (c) to room temperature, adjusting the pH value to 5.5, and filtering the solution; 6, adjusting the pH value of the filtrate to 2.5-3.0, refrigerating the filtrate overnight, carrying out suction filtration, and drying the filtrate to obtain a crude product; 7, dissolving the crude product to obtain a solution (d), and acidifying the solution(d) to an isoelectric point; 8, adding a seed crystal into the solution (d), and adjusting the solution (d) to an isoelectric point; 9, purifying a finish product. By means of the preparation method,S-carboxymethyl-L-cysteine with large particle size, high density and high purity can be obtained, and the preparation method is suitable for being used in multiple fields.

Description

technical field [0001] The invention relates to the field of amino acid preparation, in particular to a preparation method of S-carboxymethyl-L-cysteine. Background technique [0002] S-carboxymethyl-L-cysteine, alias carbocisteine, white crystalline powder; odorless, slightly soluble in hot water, insoluble in ethanol or acetone; easily soluble in acid or alkali solution. Carbocisteine ​​is a mucus thinner, which mainly affects the secretion of bronchial glands at the cellular level. It can break the disulfide bond of mucin in mucus, increase the secretion of low-viscosity sialomucin, and increase the secretion of high-viscosity rock mucin. The production of algal mucin is reduced, which reduces the viscosity of sputum and facilitates the discharge of sputum. [0003] The sites of action of carbocisteine ​​are the epithelial mucosa and mucous glands of the airway, nasal cavity, sinuses and middle ear. The epithelial mucous membranes of the respiratory tract, nasal cavity,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/14C07C323/58C07C319/28
CPCC07C319/14C07C319/28C07C323/58
Inventor 王裕祥
Owner NINGBO YUANFA BIOENG
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