A kind of esterified selenium polysaccharide and its preparation method and application
A selenium polysaccharide and esterification technology, which is applied in the field of selenium polysaccharides, can solve the problems of long reaction time, low selenium content and yield of selenized polysaccharides, and many side reactions, and achieve simple reaction conditions, adjustable selenium content, and long reaction time. short effect
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[0026] The invention provides a preparation method of esterified selenium polysaccharide, comprising the following steps:
[0027] (1) 0°C, under the protection of nitrogen, put 1 to 5 equivalents of O=SeCl 2 Add dropwise to the D-galactose allyl glycoside solution containing 1 to 5 equivalents of triethylamine, react at room temperature for 1 to 4 hours, pour into the water phase, and extract with ethyl acetate to obtain 3,4-oxo-cyclo Galactosyl allyl selenite;
[0028] (2) Suspend the polysaccharide in the solvent, add NaHCO 3 Mixing, adding acryloyl chloride dropwise to the polysaccharide solution, keeping the temperature of the reaction solution not exceeding 40°C during the dropwise addition, after the reaction is completed, dissolving the reaction solution in water and precipitating with alcohol to obtain an acrylated polysaccharide;
[0029] (3) dissolving the acrylated polysaccharide in a solvent, and undergoing a displacement reaction with 3,4-oxo-cycloselenite gala...
Embodiment 1
[0043] 0°C, under the protection of nitrogen, put 1 equivalent of O=SeCl 2 Add it dropwise to a commercially available D-galactoallyl glycoside DMSO solution containing 4 equivalents of triethylamine, react at room temperature for 4 hours, pour into the water phase, extract with ethyl acetate, wash with saturated brine, and wash the organic phase with free Dry over sodium sulfate, evaporate to dryness on a rotary evaporator under reduced pressure, and silica gel column chromatography to obtain a pure product with a yield greater than 90%.
[0044] Suspend 100 mg of β-1-3-glucan in 10 ml of anhydrous DMF, add 5 equivalents of solid sodium bicarbonate and 1 equivalent of acryloyl chloride, keep the temperature of the reaction solution not exceeding 40°C for 2 hours, and pour the reaction solution under stirring into cold water, add 4 times the volume of cold ethanol to precipitate the intermediate product, freeze-dry and set aside. The above intermediate was resuspended in dry ...
Embodiment 2
[0046] 0°C, under nitrogen protection, 5 equivalents of O=SeCl 2 Add dropwise to the D-galactoallyl glycoside DMF solution containing 2 equivalents of triethylamine, react at room temperature for 2 hours, pour into the water phase, extract with ethyl acetate, wash with saturated saline, and use anhydrous sulfuric acid for the organic phase Sodium-dried, evaporated to dryness on a rotary evaporator under reduced pressure, and silica gel column chromatography to obtain a pure product with a yield greater than 90%.
[0047] Suspend 100 mg of β-1-3-glucan in 20 ml of anhydrous DMF, add 50 equivalents of solid sodium bicarbonate and 50 equivalents of acryloyl chloride, keep the temperature of the reaction solution not exceeding 40°C for 4 hours, pour the reaction solution under stirring Put it into cold water, add 6 times the volume of cold ethanol to precipitate the intermediate product, and freeze-dry it for later use. The above intermediate was resuspended in dry DMF, 50 equiva...
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