Fluorine-containing polysaccharide high-molecular compound and preparation method thereof
A polymer compound and polysaccharide technology, which is applied in the field of fluorine-containing polysaccharide polymer compounds and its preparation, can solve the problems of poor material stability, difficult reagent deoxygenation and fluorination, and low physical strength, so as to improve stability and strength, improve Physical and chemical properties, effects of good biocompatibility
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Embodiment 1
[0047] At 70 ° C oil bath, 0.161 g of chitosan, 4 ml acetonitrile, 6 ml of 20% KOH aqueous solution, 0.225 grams of 2-fluoronacyridine-4-formic acid placed under nitrogen protection The mixture was stirred in the tube for 3 hours, and the reaction formulation is as follows:
[0048]
[0049] After completion of the reaction, cooled to room temperature, 1 mole per liter of hydrochloride system was added to the aqueous phase pH test strip. Ethyl acetate and water were added, and the resulting organic phase was added to give a saturated brine, then anhydrous magnesium sulfate was dried, carnamed dry solvent, and 0.071 g of the product was divided into a silica gel chromatography column and 44% yield.
[0050] Infrared and flu fluoroscopy were performed on the preparation product, the result was IR (Thinfilm): 3263.57, 1550.10, 1400.78, 1300.55, 1026.29CM -1 , 19 F NMR (470MHz, H 2 O, 90 ° C, δ): - 177.7 (DT, J = 55.3, 34.3 Hz), the structural formula of the preparation product is a...
Embodiment 2
[0053] At 70 ° C oil bath, 0.161 g of glycan, 4 ml acetonitrile, 6 ml of 20% KOH aqueous solution, 0.225 grams of 5-fluoronacyridine-3-formic acid under nitrogen protection The mixture was stirred in the tube for 3 hours, and the reaction formulation is as follows:
[0054]
[0055] After completion of the reaction, cooled to room temperature, 1 mole per liter of hydrochloride system was added to the aqueous phase pH test strip. Ethyl acetate and water were added, and the obtained organic phase was added to give a saturated brine, then anhydrous magnesium sulfate was dried, carnamed dry solvent, divided by silica gel chromatography column, 0.049 g, 30% yield.
[0056] Infrared and flu fluoroscopy were performed on the preparation product, the result was IR (Thinfilm): 3263.57, 1550.10, 1400.78, 1300.55, 1026.29CM -1 , 19 F NMR (470MHz, H 2 O, 90 ° C, δ): - 177.7 (DT, J = 55.3, 34.3 Hz), the structural formula of the preparation product is as follows:
[0057]
Embodiment 3
[0059] At 70 ° C oil bath temperature, 0.161 g of chitosan, 4 ml acetonitrile, 6 ml of 20% KOH aqueous solution, 0.225 grams of 2-fluoronacyridine-6-formic acid were placed under nitrogen protection The mixture was stirred in the tube for 3 hours, and the reaction formulation is as follows:
[0060]
[0061] After completion of the reaction, cooled to room temperature, 1 mole per liter of hydrochloride system was added to the aqueous phase pH test strip. Ethyl acetate and water were added, and the obtained organic phase was added to give a saturated brine, then anhydrous magnesium sulfate was dried, carnamed dry solvent, divided by silica gel chromatography column, 0.022 grams, 13% yield.
[0062] Infrared and flu fluoroscopy were performed on the preparation product, the result was IR (Thinfilm): 3263.57, 1550.10, 1400.78, 1300.55, 1026.29CM -1 , 19 F NMR (470MHz, H 2 O, 90 ° C, δ): - 177.7 (DT, J = 55.3, 34.3 Hz), the structural formula of the preparation product is as follows...
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