P-hydroxybenzene sulfonate compound as well as preparation method and application thereof

A technology of hydroxybenzenesulfonate compound and hydroxybenzenesulfonate, which is applied in the field of synthesis of hydroxybenzenesulfonate compound, and can solve problems such as lagging research work on phensulfonate and calcium dobesilate

Pending Publication Date: 2022-04-22
成都益安成贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the impurity research work of ethylamine sulfamate and calcium dobesilate lags behind

Method used

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  • P-hydroxybenzene sulfonate compound as well as preparation method and application thereof
  • P-hydroxybenzene sulfonate compound as well as preparation method and application thereof
  • P-hydroxybenzene sulfonate compound as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1 p-Hydroxybenzenesulfonic acid diethylamine salt is synthesized

[0048] Take 94.10g of phenol and add 282ml of n-heptane (3 times the volume of phenol feeding mass) and 142.10g of sulfuric acid (the amount is 1.45 equivalents of phenol), heat and stir until reflux, stir and keep warm for 4h. After the reaction is complete, remove the solvent, cool down to room temperature, add 56ml of water (0.6 times the mass volume of phenol) to disperse, then control 50-60°C and add 87.68g of diethylamine (1.2 equivalents of phenol) to form a salt. After salt formation, lower the temperature to 0-5°C, stir and heat-preserve for crystallization for 6 hours, filter with suction, wash the filter cake with 150ml of isopropanol, and dry the filter cake under vacuum at 60°C for 4 hours to obtain 209.02g of off-white powdery crude product, molar yield The rate is 84.52%.

[0049] Remove 200.04g of the crude product, add 160ml of isopropanol aqueous solution for recrystallizati...

Embodiment 2

[0051] Embodiment 2 p-Hydroxybenzenesulfonic acid calcium salt is synthesized

[0052] Take 94.23g of phenol, add 424ml of n-hexane (the amount is 4.5 times the mass volume of the phenol feed) and 147.51g of sulfuric acid (the amount is 1.5 equivalent of the phenol feed), heat and stir until reflux, stir and keep warm for 8h. Complete reaction, after being cooled to room temperature, pour off solvent, add 122.5ml into water (consumption is 1.3 times of mass volume of phenol charging capacity) after dispersing, add 114.13g calcium carbonate in batches (addition is 1.14 equivalents of phenol charging capacity) adjustment pH to 5 into a salt. After salt formation, insoluble matter was filtered off, and the filtrate was concentrated under reduced pressure at 50°C until the system was slightly turbid, and the concentration was stopped. The concentrated raffinate was cooled to 0-5°C, stirred and crystallized for 8 hours, filtered with suction, and the filter cake was rinsed with 12...

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Abstract

The invention relates to a p-hydroxybenzene sulfonate compound and application thereof, the p-hydroxybenzene sulfonate compound is specifically calcium dobesilate and etamsylate impurities, and the p-hydroxybenzene sulfonate compound is an impurity phenol brought into a starting material when hydroquinone is used as the starting material for synthesis, a process impurity generated in a sulfonation process, a process impurity generated in a sulfonation process and a process impurity generated in a sulfonation process. The compound can be used as an impurity reference substance of etamsylate bulk drugs and calcium dobesilate bulk drugs. The method disclosed by the invention has certain guiding significance on quality research of etamsylate and calcium dobesilate raw material medicines.

Description

technical field [0001] The invention relates to the field of synthesis of hydroxybenzenesulfonate compounds, in particular to an impurity of ethylamine and calcium dobesilate and its preparation method and application. Background technique [0002] Etsulfame (hemostatic) is a synthetic hemostatic drug that can reduce capillary permeability, enhance capillary resistance, constrict blood vessels, shorten bleeding time, increase platelet circulation, and increase platelet aggregation Sex and adhesion, promote the release of coagulation active substances from platelets, accelerate the shrinkage of blood clots, and are commonly used hemostatic drugs in clinical practice. The hemostatic effect of Etsulfametamine is rapid and can last for 4 to 6 hours. It is suitable for the prevention and treatment of excessive surgical bleeding, thrombocytopenic purpura or allergic purpura and bleeding caused by other reasons, such as: cerebral hemorrhage, gastrointestinal bleeding, Urinary trac...

Claims

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Application Information

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IPC IPC(8): C07C309/42C07C303/32C07C303/44C07C209/00C07C211/05
CPCC07C309/42C07C303/32C07C303/44C07C303/06C07C303/08C07C209/00C07C211/05
Inventor 倪瑛陈巍刘鹏
Owner 成都益安成贸易有限公司
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