Method for synthesizing Artemisia sphaerocephala polysaccharide derivatives by adopting acidic ionic liquid as catalyst
A technology of acidic ionic liquid and polysaccharide derivatives is applied in the field of application of selenized Artemisia annua polysaccharide to inhibit H1650 lung cancer cells in vitro, and can solve the problems of unfavorable molecular weight and molecular weight distribution, complex preparation of selenium-containing intermediates, unfriendly environment and the like. , to achieve the effect of shortening the time required for the reaction, high yield, and reducing the acid hydrolysis reaction steps
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Embodiment 1
[0044] A kind of synthesis of polysaccharide of selenized Artemisia annua, comprising:
[0045] (1) Preparation of polysaccharide formamide solution: 300 mg polysaccharide polysaccharide was dissolved in 75 mL anhydrous formamide at 60°C and 800 rpm for 3 h to obtain the polysaccharide formamide solution.
[0046] (2) Preparation of acidic ionic liquid: Add 10 mL concentrated nitric acid dropwise to 9.86 g imidazole at a rate of 40 drops / min at -10°C. After completion, wash with 10 mL ethyl acetate for 5 times at room temperature, collect the lower layer, and vacuum-dry at 70 °C and 0.06 MPa for 9 h to obtain an acidic ionic liquid. H 0 is 3.78.
[0047] (3) Synthesis of polysaccharides from selenized Artemisia argyi: 0.75 g of selenous acid was added to 10 mL of acidic ionic liquid prepared in step (2), and the 2 Under the condition of protection, add the formamide solution of Artemisia polysaccharides in (1) dropwise at a rate of 80 drops / min with a dropping funnel. Afte...
Embodiment 2
[0050] A kind of synthesis of polysaccharide of selenized Artemisia annua, comprising:
[0051] (1) Preparation of polysaccharide formamide solution: 300 mg polysaccharide polysaccharide was dissolved in 150 mL anhydrous formamide at 70°C and 500 rpm for 6 h to obtain the polysaccharide formamide solution.
[0052] (2) Preparation of acidic ionic liquid: 10 mL of concentrated sulfuric acid was added dropwise to 15.1 g of methylimidazole at a rate of 50 drops / min at 0 °C. After the addition was completed, the reaction was stirred at room temperature at 700 rpm for 12 h. After the reaction was completed, it was washed three times with 15 mL of ethyl acetate at room temperature, and the lower layer was collected and vacuum-dried at 50 °C and 0.07 MPa for 12 h to obtain an acidic ionic liquid. H 0 is 3.76.
[0053] (3) Synthesis of polysaccharides from selenized Artemisia arvensis: 0.75 g of selenous acid was added to the acidic ionic liquid (12.5 mL) prepared in step (2), unde...
Embodiment 3
[0056] A kind of synthesis of polysaccharide of selenized Artemisia annua, comprising:
[0057] (1) Preparation of polysaccharide formamide solution: 300 mg polysaccharide polysaccharide was dissolved in 100 mL anhydrous formamide at 50°C and 600 rpm for 5 h to obtain the polysaccharide formamide solution.
[0058] (2) Preparation of acidic ionic liquid: Add 10 mL of concentrated hydrochloric acid dropwise to 8.16 g of imidazole at a rate of 60 drops / min at -5°C. After completion, wash with 10 mL of ethyl acetate four times at room temperature, collect the lower layer, and vacuum-dry at 60 °C and 0.08 MPa for 8 h to obtain an acidic ionic liquid. H 0 was 3.79.
[0059] (3) Synthesis of polysaccharides from selenized Artemisia arvensis: 0.75 g of selenous acid was added to the acidic ionic liquid (7.5 mL) prepared in step (2), and the 2 Under the condition of protection, add the formamide solution of Artemisia polysaccharides in (1) dropwise at a rate of 70 drops / min with a...
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