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Method for producing high-purity etamsylate

A high-purity technology of ethylamine, which is applied in the field of preparation of ethylamine, can solve the problems of unfriendly environment and high toxicity of ethylamine, and achieve the goals of shortening post-processing time, simplifying operation and reducing energy consumption Effect

Active Publication Date: 2019-03-15
云南元顺医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the technical defects of high toxicity and unfriendly environment in the preparation of ethylamine in the prior art, the present invention provides a method for producing high-purity ethylamine, which improves the fluidity of the reaction system, improves the product purity, and improves the product purity. Reaching more than 99.5%, the solvents used are all changed to second-class and third-class solvents that are safe, low-toxic, and more friendly to humans and the environment

Method used

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  • Method for producing high-purity etamsylate
  • Method for producing high-purity etamsylate
  • Method for producing high-purity etamsylate

Examples

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Effect test

Embodiment 1

[0030] Add 1.65kg of hydroquinone, 4.5L of n-heptane, and 0.22L of glacial acetic acid into a 10L enamel reaction kettle, stir and heat up to reflux, reflux and divide water for 2 hours, after water separation, cool down to slight reflux, that is, control the temperature in the enamel reaction kettle. temperature to 80°C, add 2.28kg of concentrated sulfuric acid, and control the internal temperature to not exceed 90°C. After the addition is complete, keep warm at 85°C, and react with slight reflux for 30 minutes. Stop heating, pass in cooling water to lower the temperature of the paste in the lower layer to 45°C, and drop in 1.42 The mixed solution of kg diethylamine and 0.99L water is added dropwise at an internal temperature of 55°C. After the drop is completed, the temperature is raised to 65°C and stirred to dissolve the lower aqueous phase. Cool down to 10°C, keep stirring and crystallize for 1h. Then lower the temperature to 0°C, heat preservation, stir and crystallize f...

Embodiment 2

[0032] Add 1.65kg of hydroquinone, 4.2L of n-hexane, and 0.2L of acetic anhydride into a 10L enamel reaction kettle, stir and heat up to reflux, reflux and divide water for 1 hour, after water separation, cool down to microreflux, and control the internal temperature of the microreflux reactor 70°C, add 1.9kg of concentrated sulfuric acid, control the internal temperature of the reactor to not exceed 75°C, after the addition is complete, keep warm for 50 minutes under reflux, stop heating, pass in cooling water to lower the temperature of the paste in the lower layer to 50°C, and drop 1.4kg of di For the mixture of ethylamine and 0.9L water, add dropwise at an internal temperature of 50°C, and the maximum temperature should not exceed 70°C. After dropping, raise the temperature to 70°C and stir to dissolve the lower aqueous phase. Reactor, slowly cool down to about 10°C, keep stirring and crystallize for 1 hour, then cool down to 3°C, keep stirring and crystallize, then dischar...

Embodiment 3

[0034] Add 1.65kg of hydroquinone, 4.5L of cyclohexane, and 0.2L of propionic acid into a 10L enamel reaction kettle, stir and raise the temperature to reflux, and reflux to separate water for 2 hours. After the water separation is completed, the temperature is lowered to a slight reflux. The inner temperature of the micro-reflux reactor is 85°C, and 2.28kg of concentrated sulfuric acid is added to control the inner temperature of the reactor to not exceed 90°C; Put in cooling water to lower the temperature of the paste in the lower layer to 65°C, add a mixture of 1.25kg of diethylamine and 0.9L of water dropwise, control the inner temperature of the reactor at 65°C, and the maximum temperature of the reactor should not exceed 70°C; Stir to 70°C to dissolve the lower water phase, and separate the liquid while it is hot; collect the water phase, transfer it to a 10L reactor, slowly cool down to about 10°C, keep stirring and crystallize for 1 hour, then cool down to 5°C, keep sti...

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Abstract

The invention discloses a method for producing high-purity etamsylate. The method comprises the following steps: carrying out a sulfonation reaction on hydroquinone serving as an initial material, a sulfonating agent, a dispersing agent and an organic solvent to obtain 2,5-dihydroxybenzenesulfonic acid; cooling the reaction solution to 45-70 DEG C, adding a mixed solution of diethylamine and waterto form a salt, cooling and crystallizing, so as to obtain the etamsylate. According to the reaction system used in the method, the fluidity of the system is improved, and the three-transfer-one-reaction efficiency is improved, so that the conversion rate of the materials is improved by 5-10%; when the system is cooled to 45-70 DEG C after the reaction is ended, the mixed solution of diethylamineand water is directly added into the system, the operation is simplified, and the after-treatment time is shortened; concentrated water is avoided, the energy consumption is reduced, and the yield ofthe product after salt formation reaches 80-85%; the product does not need to be re-crystallized or subjected to activated carbon discoloration, the purity directly reaches 99.5% or higher, and the content of all single impurities is lower than 0.05%; in addition, the use of a type of solvents and reagents containing genotoxicity warning structures is avoided, and totally safe and low-toxicity class-2 and class-3 solvents friendly to the humans and environment are used.

Description

technical field [0001] The invention relates to the field of preparation of phensulfame, in particular to a method for producing high-purity phensulfame. Background technique [0002] Etamsulfame, commonly known as hemostatic, is a synthetic hemostatic drug that can reduce capillary permeability, enhance capillary resistance, constrict blood vessels, shorten bleeding time, increase platelet circulation, increase platelet Aggregation and adhesion promote the release of coagulation active substances from platelets and accelerate the shrinkage of blood clots. It is a commonly used hemostatic drug 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 tract bleeding, fundus bleeding, gum bleeding, epistaxis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/06C07C309/42C07C209/00C07C211/05
CPCC07C209/00C07C303/06C07C309/42C07C211/05
Inventor 靳磊卢杰倪瑛张玲张为群
Owner 云南元顺医药有限公司
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