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A kind of synthetic method of carbocisteine

A synthetic method and technology of carbocisteine, which is applied in the field of synthesis and production of carbocisteine, can solve problems such as difficult operation, harsh reaction conditions, and many equipment configurations, and achieve the effect of reducing material consumption and energy consumption

Active Publication Date: 2017-09-05
宜昌三峡普诺丁生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the deficiencies in the prior art such as complicated process, many equipments, harsh reaction conditions, difficult operation and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 600 liters of purified water to the reaction tank, add 250 kg of cysteine ​​hydrochloride monohydrate and 140 kg of chloroacetic acid under stirring, and stir until completely dissolved; add sodium hydroxide solution to the reaction tank, and control the addition of Speed ​​and open cooling water cooling, control the temperature of the reaction solution to be 30°C, add flow until the pH value of the reaction solution reaches 8.5, and react for 1 hour. It is weakly positive to detect cysteine ​​with the color reaction, add 1.5 kg of chloroacetic acid, add Adjust the pH value of the sodium hydroxide solution to 8.5 and continue the reaction for 0.5 hours, and then detect that cysteine ​​is negative; add concentrated hydrochloric acid to the reaction solution to adjust the pH value to 6.5, heat to 65 ° C, add 2 kg of activated carbon, and stir for 1 hour to decolorize. Heat with a filter and filter in the crystallization tank; add concentrated hydrochloric acid to the c...

Embodiment 2

[0034] Add 620 liters of purified water into the reaction tank, add 225 kg of cysteine ​​hydrochloride anhydrate and 140 kg of chloroacetic acid under stirring, and stir until completely dissolved; add sodium hydroxide solution to the reaction tank, and control the addition of Speed ​​and open cooling water cooling, control the temperature of the reaction solution to be 30°C, add flow until the pH value of the reaction solution reaches 8.5 and then react for 1 hour. It is weakly positive to detect cysteine ​​with the color reaction, add 2 kg of chloroacetic acid, add Adjust the pH value of the sodium hydroxide solution to 8.5 and continue the reaction for 0.5 hours, and then detect that cysteine ​​is negative; add concentrated hydrochloric acid to the reaction solution to adjust the pH value to 6.5, heat to 70 ° C, add 2 kg of activated carbon, and stir for 0.5 hours to decolorize. Heat with a filter and filter in the crystallization tank; add concentrated hydrochloric acid to ...

Embodiment 3

[0036] Add 150 liters of purified water in the reaction tank, drop into 171 kilograms of cystine under agitation and be the cysteine ​​hydrochloride reaction liquid that the starting material makes through reduction reaction, 140 kilograms of chloroacetic acid, stir until all dissolving; Add sodium hydroxide solution to the reaction tank, control the adding speed and turn on the cooling water to cool, control the temperature of the reaction solution to 30°C, add the solution until the pH value of the reaction solution reaches 8.5, and react for 1 hour, and use the color reaction to detect cysteamine The acid is negative; add concentrated hydrochloric acid to the reaction solution to adjust the pH value to 6.5, heat to 70°C, add 3 kg of activated carbon, stir and decolorize for 0.5 hours, then filter it into the crystallization tank while it is hot; pour it into the crystallization tank under stirring Add concentrated hydrochloric acid to neutralize the decolorization solution u...

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Abstract

The invention relates to a synthetic method of carbocisteine, wherein a two-pot reaction process in the prior art is changed into a one-pot reaction process, thereby simplifying the process and reducing devices. A low-temperature nitrogen protective process is changed into a normal-temperature nitrogen-free protective process, thereby reducing material and energy consumptions. A two-step crystallization process is changed into a one-step crystallization process, thereby reducing processes and devices and increasing the yield.

Description

technical field [0001] The invention relates to a method for synthesizing and producing carbocisteine. Background technique [0002] Carbocisteine ​​is an expectorant and cough medicine that is safe, rapid, efficient, widely applicable, and has few side effects. It is mainly used for thick sputum, difficulty in coughing up sputum, and obstructed trachea caused by chronic bronchitis, bronchial asthma and other diseases. Treatment of other diseases. [0003] There are many production processes of carbocisteine, and different starting materials can be used to obtain the final product through different process routes, but the most direct synthetic reaction is to use cysteine ​​hydrochloride and chloroacetic acid as raw materials in weak The carboxylation reaction is carried out under alkaline conditions. The existing common process is to neutralize cysteine ​​hydrochloride and chloroacetic acid with alkali to form a neutral to weakly alkaline solution, and then mix the two unde...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/58C07C319/20C07C319/28
CPCC07C319/20C07C319/28C07C323/58
Inventor 江兵邓强胡燕陈光喜程霞
Owner 宜昌三峡普诺丁生物制药有限公司
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