Cationic polyhydroxylated polymer embolization microspheres and preparation method thereof
A polyhydroxy polymer and embolizing microsphere technology, applied in microcapsules, drug delivery, pharmaceutical formulations, etc., can solve the problems of easy generation of drug resistance, reducing the density of cationic groups, and obtaining a good therapeutic effect, etc. Avoid tumor multidrug resistance, avoid strong cytotoxicity, and increase the effect of cation density
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Embodiment 1
[0036] Dissolve 40 g of NaOH in 300 mL of purified water, stir and dissolve at 250 rpm, and cool down to 1 °C with an ice-salt bath. Then 147.3 g of aminoacetaldehyde diethyl acetal were added slowly. After the system was uniform, 99.5 g of acryloyl chloride was slowly added dropwise, and after the dropwise addition was completed, the reaction was kept at 5°C for 30 min. Then add 150 mL saturated sodium chloride solution to the above solution, add methyl tert-butyl ether for extraction after stirring completely. The oily liquid in the upper layer was collected, and the crude product obtained after concentration was purified by column chromatography to obtain N-acrylamidodiethoxy acetal (95.7 g) as a colorless and transparent oily product.
Embodiment 2
[0038] Dissolve 30 g of NaOH in 300 mL of purified water, stir and dissolve at 280 rpm, and cool down to 10 °C with an ice-salt bath. Then 100.2 g of 4-aminobutyraldehyde dimethyl acetal were added slowly. After the system was uniform, 67.5 g of acryloyl chloride was slowly added dropwise, and after the dropwise addition was completed, the reaction was kept at 10°C for 30 min. Then add 100 mL saturated sodium chloride solution to the above solution, add methyl tert-butyl ether for extraction after stirring completely. The oily liquid in the upper layer was collected, and the crude product obtained after concentration was purified by column chromatography to obtain N-acrylamidodimethoxybutyral (64.2 g) as a colorless and transparent oily product.
[0039] Synthesis of Functionalized Polyol Intermediates
Embodiment 3
[0041] Measure 180 g of polyvinyl alcohol, add 1000 mL of purified water into a 2 L reaction flask, stir and dissolve at a temperature of 90 °C and a speed of 200 rpm. After the solid was completely dissolved and the system was cooled to room temperature, 2.93 g of the small molecule cross-linking agent N-acrylamide diethoxy acetal and 13.3 g of aminoacetaldehyde diethyl acetal were added to it, and after stirring for 10 minutes, Add 100mL of 36% hydrochloric acid dropwise. After the dropwise addition, the mixture was incubated at 15°C for 6 hours. After the reaction, the system was adjusted to pH 7.0 with 1.5 mol / L sodium hydroxide solution and stabilized for 10 minutes. Then collect the crude product, remove impurities by suction filtration, and concentrate to obtain the desired functionalized polyhydroxy polymer intermediate, and the viscosity is controlled at 1500 cps.
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