FIELD: chemistry.
SUBSTANCE: in the proposed method, 7-monohydroxyethyl rutoside is first produced by ethylation of the routine followed by purification, and then converted to trihydroxyethyl rutoside by hydroxyethylation. At the stage of producing 7-monohydroxyethyl rutoside, hydroxyl routine groups are protected with a hydroxyl protecting agent, the hydroxyl-protecting agent is borax, the hydroxyethylating agent is ethylene oxide, the solvent is selected from water, methanol and ethanol, the reaction temperature is 30-50°C, and the time is 4-14 hours; for purifycation, re-crystallization from water, methanol, ethanol, isopropanol and mixtures thereof is used; at the stage of producing trihydroxyethyl rutoside of purified 7-monohydroxyethyloxy rutoside, the hydroxyethylating agent is added after dissolving or dispersing 7-monohydroxyethyloxy rutoside in the solvent, where the hydroxyethylating agent is ethylene oxide, the solvent is selected from water, methanol, ethanol, pyridine and mixtures thereof, the catalyst is selected from sodium hydroxide, potassium hydroxide and ammonia water, the reaction temperature is 50-80° and the reaction time is 3-8 hours, and the product is passed through cationic and anionic resin or treated with macroporous resin after completion of the reaction; where the said cationic resins are selected from strongly acidic polystyrene cation exchange resins, the anionic resins are selected from strongly basic polystyrene anion exchange resins; where the said macroporous resins are selected from nonpolar macroporous polystyrene resins and low-polar macroporous resins; at the stage of purifying trihydroxyethyl rutoside for purification, the re-recrystallization is used, where the solvent for re-crystallization is selected from water, methanol, ethanol, isopropanol and mixtures thereof, further the product purification is carried out to ensure that 7,3',4'-trihydroxyethyl rutoside is produced with a degree of purity greater than 98 wt %.
EFFECT: new efficient method of producing a valuable product with a high degree of purity.
8 cl, 6 dwg, 11 ex
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Authors
Dates
2017-11-29—Published
2014-05-23—Filed