- C10H17NO5S.1/20H2O compound
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The invention discloses a C10H17NO5S.1/20H2O compound and a preparation method thereof. The compound is measured by using a powder X-ray diffraction measurement method, and shows characteristic diffraction peaks represented by a diffraction angle of 2theta +/- 0.2 degrees at the places of 13.4 degrees, 17.2 degrees, 20.5 degrees, 21.4 degrees, 23.7 degrees, 24.5 degrees, 26.9 degrees, 28.0 degreesand 34.0 degrees. The C10H17NO5S.1/20H2O compound prepared by the preparation method has the advantages of good thermal stability, high purity, and weak hygroscopicity, has a simple process, a high yield and strong repeatability, and is suitable for industrial production.
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- Method for producing high-purity etamsylate
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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.
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Paragraph 0025; 0029-0036
(2019/03/29)
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