A kind of preparation technology of carbocisteine

A technology for preparing carbocisteine, which is applied in the field of organic synthesis, can solve the problems of difficult intermediate process control, unsatisfactory purity, and low yield of carbocisteine, and achieve easy operation and control, good stability, The effect of high purity

Active Publication Date: 2017-11-03
LUOJIANG CHENMING BIOLOGICAL PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disclosed in CN103102294A is a kind of synthetic method that utilizes L-cysteine ​​hydrochloride monohydrate and liquid chloroacetic acid to carry out carbocisteine, but the yield of carbocisteine ​​is low under this process condition, and the purity is not enough Ideal, but it is difficult to control the intermediate process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The preparation technology of the carbocisteine ​​of the present embodiment is realized through the following steps:

[0033] (a) Take L-cysteine ​​hydrochloride monohydrate and solid chloroacetic acid, wherein, L-cysteine ​​hydrochloride monohydrate is 150KG, chloroacetic acid is L-cysteine ​​hydrochloride 60% of the amount of monohydrate, that is, 90KG;

[0034] (b) Put the reactants L-cysteine ​​hydrochloride monohydrate and chloroacetic acid into the reaction kettle, add 600KG of water and stir to dissolve, and heat during the dissolution process to control the temperature of the system at about 20°C;

[0035] (c) Use liquid ammonia and add ammonium bicarbonate at the same time to adjust the pH of the system to 7.5. The amount of ammonium bicarbonate added is 200KG, and the temperature of the system is controlled at 45-50°C, and the reaction is stirred for 30 minutes;

[0036] (d) After the reaction is completed, adjust the pH of the system to 6.0 with hydrochloric...

Embodiment 2

[0040] The preparation technology of the carbocisteine ​​of the present embodiment is realized through the following steps:

[0041] (a) Take L-cysteine ​​hydrochloride monohydrate and solid chloroacetic acid, wherein, L-cysteine ​​hydrochloride monohydrate is 150KG, chloroacetic acid is L-cysteine ​​hydrochloride 60% of the amount of monohydrate, that is, 90KG;

[0042] (b) Put the reactants L-cysteine ​​hydrochloride monohydrate and chloroacetic acid into the reaction kettle, add 600KG of water and stir to dissolve, and heat during the dissolution process to control the temperature of the system at about 20°C;

[0043] (c) Use liquid ammonia to adjust the pH of the system to 7.5, control the temperature of the system to 45-50°C, and react for 30 minutes in a stirring state;

[0044] (d) After the reaction is completed, adjust the pH of the system to 6.0 with hydrochloric acid, and add 20kg of activated carbon for decolorization and adsorption of impurities. During the proce...

Embodiment 3

[0048] The preparation technology of the carbocisteine ​​of the present embodiment is realized through the following steps:

[0049] (a) Take L-cysteine ​​hydrochloride monohydrate and solid chloroacetic acid, wherein, L-cysteine ​​hydrochloride monohydrate is 150KG, chloroacetic acid is L-cysteine ​​hydrochloride 70% of the amount of monohydrate, that is, 105KG;

[0050] (b) Put the reactants L-cysteine ​​hydrochloride monohydrate and chloroacetic acid into the reaction kettle, add 450KG of water and stir to dissolve, and heat during the dissolution process to control the system temperature at about 25°C;

[0051] (c) Use liquid ammonia and add ammonium bicarbonate at the same time to adjust the pH of the system to 7.5. The amount of ammonium bicarbonate added is 210KG. At the same time, the temperature of the system is controlled at 45-50°C, and the reaction is stirred for 90 minutes;

[0052] (d) After the reaction is completed, adjust the pH of the system to 6.4 with hydr...

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PUM

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Abstract

The invention discloses a preparation process of a compound, in particular to a preparation process of carbocisteine, and belongs to the technical field of organic synthesis. The preparation method includes following steps: (a), taking L-cysteine hydrochloride monohydrate and solid chloroacetic acid, wherein chloroacetic acid accounts for 60-70% of mass of L-cysteine hydrochloride monohydrate; (b), adding water into L-cysteine hydrochloride monohydrate and chloroacetic acid, stirring for dissolution, and controlling temperature of a system to 15-25 DEG C in the process of dissolution; (c), adjusting PH of the system to 7.0-7.5, controlling temperature of the system to 45-50 DEG C, and stirring and allowing reaction; (d), after reaction is completed, adjusting PH of the system to 6.0-6.4, and performing decoloring and impurity adsorption treatment; (e), filtering, adjusting PH of filtrate to 2.8-3.0, and cooling to obtain carbocisteine. Carbocisteine prepared by the preparation process has the advantages of high purity, high yield and high stability, and the preparation process is simple and easy to operate and control.

Description

technical field [0001] The invention relates to a preparation process of a compound, in particular to a preparation process of carbocisteine, belonging to the technical field of organic synthesis. Background technique [0002] Carbocisteine ​​is a medicine mainly used for the treatment of thick sputum, difficulty in coughing up sputum, and obstructed trachea caused by phlegm caused by chronic bronchitis, bronchial asthma and other diseases. At the same time, carbocisteine ​​is also an important pharmaceutical intermediate and chemical raw material. [0003] Carbocisteine ​​has multiple synthetic routes and synthetic methods, one of which is to use L-cysteine ​​hydrochloride monohydrate and chloroacetic acid as raw materials for synthesis. Disclosed in CN103102294A is a kind of synthetic method that utilizes L-cysteine ​​hydrochloride monohydrate and liquid chloroacetic acid to carry out carbocisteine, but the yield of carbocisteine ​​is low under this process condition, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/14C07C319/28C07C323/58
CPCC07C319/14C07C319/28C07C323/58
Inventor 谢启明谢宏秋
Owner LUOJIANG CHENMING BIOLOGICAL PROD
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