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Preparation method of sodium gualenate

A technology of sodium azulene sulfonate and sulfonating agent is applied in directions such as sulfonic acid preparation, sulfonate preparation, chemical instrument and method, and can solve the problems of high preparation cost, difficult to obtain raw materials, unfavorable large-scale production and application, etc., Achieve the effect of low production cost and simple steps

Inactive Publication Date: 2018-11-23
西安宇泰药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above-mentioned situation, the purpose of the present invention is to solve the problems in the prior art that the existing steps for preparing sodium azulene sulfonate are relatively cumbersome, and the raw materials are not easy to obtain, the preparation cost is high, and it is unfavorable for large-scale production and application.

Method used

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  • Preparation method of sodium gualenate
  • Preparation method of sodium gualenate
  • Preparation method of sodium gualenate

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Embodiment 1

[0030] In order to solve this technical problem, the present invention proposes a kind of preparation method of sodium azulene sulfonate, please refer to figure 1 , for the preparation method of sodium azulene sulfonate that the first embodiment of the present invention proposes, comprise the steps:

[0031] (1) Preparation of sulfonating agent

[0032] Dichloroethane and triethyl phosphate are sequentially added into the reaction pot, sulfur trioxide is introduced under the condition of stirring, and the sulfonating agent is prepared at the first preset temperature.

[0033] In this step, sulfur trioxide is fed through a flow meter, and the above-mentioned first preset temperature is 0°C.

[0034] (2) Sulfonation synthesis: add guaiazulene and ethylene dichloride into the reaction pot, and add the sulfonating agent dropwise to In the reaction pot, after the dropwise addition is completed, the temperature is controlled to be lower than the third preset temperature for the fi...

Embodiment 2

[0040] The preparation method of sodium azulene sulfonate proposed by the present invention is described in more detail below with a specific embodiment. Specifically, see figure 2 , the preparation method in this embodiment is specifically as follows:

[0041] (1), preparation of sulfonating agent

[0042] Put dichloroethane and triethyl phosphate into the reaction pot respectively, turn on the stirring device, and slowly introduce sulfur trioxide. Specifically, the sulfonating agent is prepared at 0° C. by feeding it through a flow meter according to the ratio for use in the next process.

[0043] (2), sulfonation synthesis

[0044] Put guaiazulene and dichloroethane into the reaction pot in proportion, turn on the stirring device to stir, and when the temperature of the material is -5°C, vacuum pump the sulfonating agent prepared in the above steps, and slowly introduce it at a controlled speed , Keep the reaction for half an hour in an environment lower than 10°C afte...

Embodiment 3

[0052] In the present invention, also propose a kind of preparation method of guaiacene, please refer to image 3 , including the following steps:

[0053](1) Turn on the vacuum equipment of the hydrogenation reactor, open the valve of the suction port, and inhale the orangerene into the reactor. Specifically, the raw material barrel is placed on the electronic scale, and the amount of raw material added is calculated through the reading change. After the suction is completed, turn off the vacuum equipment, turn on the stirring under normal pressure, start the suction port above the reactor, open the feed port above the reactor, add Raney nickel, close the feed port after feeding, and close the suction port above the reactor. tuyere.

[0054] (2) After the feeding process is over, replace the air in the kettle with hydrogen, then inject hydrogen into the reactor to 0.3MPa, turn on the steam for heating, control the temperature in the reactor to 130°C, and keep the hydrogen i...

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Abstract

The invention provides a preparation method of sodium gualenate. The preparation method comprises the following steps: preparing a sulfonating agent: adding dichloroethane and triethyl phosphate intoa reaction pot in sequence; under a stirring condition, introducing sulfur trioxide; preparing the sulfonating agent at first pre-set temperature; carrying out sulfonating synthesis: adding guaiazulene and the dichloroethane into the reaction pot; dropwise adding the sulfonating agent into the reaction pot through a vacuum negative-pressure manner at second pre-set temperature under a stirring condition; after finishing dropwise adding, controlling the temperature to be less than third pre-set temperature and reacting for first pre-set time; continually adding alkali liquid into the reaction pot; after sufficiently stirring, freezing to obtain a frozen material; refining sodium sulfonate: adding the frozen material and distilled water into a refining pot according to a pre-set ratio; filtering impurities at fourth pre-set temperature; centrifuging and drying under a room-temperature environment to finally obtain the sodium gualenate. The preparation method provided by the invention hasthe advantages that raw materials are easy to obtain and large-scale production and application can be realized.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of sodium azulene sulfonate. Background technique [0002] In daily life, people are prone to inflammation in the body due to various external factors. If it is not dealt with in time, it will cause more damage. [0003] When performing anti-inflammatory treatment, it is inevitable to use anti-inflammatory and bactericidal drugs. Pharyngitis is a common inflammation, and patients need to take pharyngitis drugs for anti-inflammatory treatment. Sodium azulene sulfonate, as a common pharyngitis drug, has a good effect on controlling patients' pharyngitis. [0004] However, the existing steps for preparing sodium azulene sulfonate are relatively cumbersome, and the raw materials are not easy to obtain, and the preparation cost is high, which is not conducive to large-scale production and application. Contents of the invention [0005] In view of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/25C07C303/06C07C303/32C07C1/24C07C13/54C07C5/373C07C13/52
CPCC07C1/24C07C5/373C07C303/06C07C303/32C07C2602/26C07C2603/30C07C13/54C07C13/52C07C309/25
Inventor 李国进
Owner 西安宇泰药业有限公司
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