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Preparation method of phloroglucinol

A technology for phloroglucinol and resorcinol, which is applied in the field of chemical material preparation, can solve problems such as difficulty in extraction, and achieve the effects of shortening reaction time, reducing production cost and reducing pollution

Active Publication Date: 2014-03-19
KAIFENG MINGREN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Flavonoid derivatives widely exist in natural plants, but extraction is difficult

Method used

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  • Preparation method of phloroglucinol
  • Preparation method of phloroglucinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The preparation method of phloroglucinol of the present invention, the detailed steps of described preparation method are as follows:

[0033] a, bromination reaction: with resorcinol as raw material, first resorcinol is added in the reaction vessel, then chloroform is added for dissolving, after dissolving, N-bromosuccinimide is dissolved in chloroform to obtain N -The bromosuccinimide solution was added dropwise to the reaction container, and the N-bromosuccinimide solution was added dropwise for 30 minutes. After the dropwise addition, the temperature was raised to 60°C, and the reaction was carried out at this temperature for 1 hour. Finally, the reaction liquid was obtained, and the obtained reaction liquid was distilled out of chloroform at normal pressure, and the obtained liquid was distilled under reduced pressure, and the 150-160 ° C fraction was collected under a vacuum degree of 0.098 MPa, and the obtained fraction was cooled to normal temperature to obtain 4...

Embodiment 2

[0040] The preparation method of phloroglucinol of the present invention, the detailed steps of described preparation method are as follows:

[0041] a. Bromination reaction: using resorcinol as raw material, first add resorcinol into the reaction vessel, then add dichloromethane to dissolve, and dissolve N-bromosuccinimide in dichloromethane The N-bromosuccinimide solution obtained in is added dropwise to the reaction vessel, and the time for adding the N-bromosuccinimide solution is 35 minutes. After the dropwise addition, the temperature is raised to 40°C. Reaction for 3 hours, after the reaction, the reaction solution was obtained, and dichloromethane was distilled from the obtained reaction solution under normal pressure, and the obtained liquid was distilled under reduced pressure, and the fraction at 150-160°C was collected under a vacuum degree of 0.098MPa, and the obtained fraction was distilled Cool to normal temperature to obtain 4-bromoresorcinol;

[0042] The rat...

Embodiment 3

[0048] The preparation method of phloroglucinol of the present invention, the detailed steps of described preparation method are as follows:

[0049] a, bromination reaction: with resorcinol as raw material, first resorcinol is added in the reaction vessel, then acetone is added to dissolve, after dissolution, N-bromosuccinimide is dissolved in acetone to obtain N -The bromosuccinimide solution was added dropwise to the reaction container, and the N-bromosuccinimide solution was added dropwise for 40 minutes. After the dropwise addition, the temperature was raised to 80°C, and the reaction was carried out at this temperature for 0.5h. After the reaction, the reaction liquid was obtained, and the obtained reaction liquid was distilled to remove acetone under normal pressure. After the acetone was distilled off, the obtained liquid was distilled under reduced pressure, and the 150-160 ° C fraction was collected under a vacuum of 0.098 MPa, and the obtained fraction was cooled to ...

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Abstract

The invention discloses a preparation method of phloroglucinol, which comprises the following steps: dissolving resorcinol in reaction solvent, then adding an N-bromosuccinimide solution, heating to perform bromination reaction, and then treating to obtain 4-bromoresorcinol; adding the obtained 4-bromoresorcinol into a container, adding reaction solvent, strong alkali and a catalyst, heating to perform hydrolysis reaction, and then treating to obtain a phloroglucinol salt solution; and adding hydrochloric acid into the phloroglucinol salt solution to regulate the pH value and precipitate solid, filtering to obtain the solid phloroglucinol crude product, and finally purifying to obtain the phloroglucinol product. According to the preparation method, the low-price accessible resorcinol is used as the raw material and is subjected to bromination, strong alkali hydrolysis and acidification, thus preparing the phloroglucinol. According to the invention, the reaction time is shortened, the production cost is lowered, and remarkable economic benefits are achieved. By preparing the phloroglucinol through the preparation method, the yield is up to 70% or above, and the purity of the prepared product is up to 99.9% or above.

Description

technical field [0001] The invention relates to a preparation method of phloroglucinol, which belongs to the technical field of chemical material preparation, in particular to a method for preparing phloroglucinol with resorcinol as a basic raw material. Background technique [0002] Phloroglucinol (1,3,5-trihydroxybenzene) is an important fine chemical product, mainly used as an intermediate in pharmaceutical synthesis, such as flavonoids. As drugs for the treatment of cardiovascular and cerebrovascular diseases, flavonoids have attracted more and more attention from pharmacologists. Flavonoid derivatives widely exist in natural plants, but it is difficult to extract them. Designing and synthesizing effective drugs using brass as a matrix has become a research hotspot, among which there are quite a few drugs synthesized using phloroglucinol as a raw material. Western countries such as Europe have taken the lead in the world in such drugs, and most of them are in the resea...

Claims

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Application Information

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IPC IPC(8): C07C39/10C07C37/02
CPCC07C37/02C07C37/62C07C39/10C07C39/245
Inventor 李沁沁朱赞梅黄振阳王艳桥翟腾苗海敏
Owner KAIFENG MINGREN PHARMA
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