Visual polyhydroxy polymer embolism microsphere and preparation method thereof
A technology of embolic microspheres and polymers, applied in the field of medical materials, can solve the problems of increased difficulty, cumbersome operation steps, and vascular stimulation, and achieve the effects of simple operation, reduced surgical risk, and good scalability
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[0036] Example 1
[0037]
[0038] Slowly add 50mL of dimethyl sulfoxide solution containing 419.0g of 3,5-diiodo-4-aminobenzaldehyde dimethyl acetal to a four-necked reaction flask containing an aqueous sodium hydroxide solution (40g, 300mL), and stir to make the solution Uniform; slowly add acryloyl chloride (99.5g) dropwise, and continue the reaction for 1 hour after the dropwise addition is complete. Then, saturated sodium chloride solution (100mL) was added to the above solution, ethyl acetate (2×200mL) was added for extraction, the organic phase was washed with water (2×100mL), and the crude product obtained after concentration of the organic phase was purified by column chromatography to obtain light Yellow oily product 3,5-diiodo-4-acrylamido benzaldehyde dimethyl acetal 1 (300g), HPLC purity 99.0%, 1 HNMR[DMSO-d 6 ]: 8.201 (s, 1H), 7.541 (s, 2H), 6.482-6.410 (m, 1H), 6.172-6.124 (m, 1H), 5.714-5.682 (m, 1H), 5.490 (s, 1H), 3.252(s, 6H).
Example Embodiment
[0039] Example 2
[0040]
[0041] In a 2L four-necked reaction flask, add 1000g of water and the molecular weight is 5×10 4 ~8×10 4 150g of polyvinyl alcohol, heated to 96°C for 4 hours, cooled the fully dissolved polyvinyl alcohol solution to room temperature, and added 15.7g of 3,5-diiodo-4-acrylamidobenzaldehyde dimethylacetal 10 mL of dimethyl sulfoxide solution and 100 mL of concentrated hydrochloric acid were reacted for 3 hours. After the reaction, 560 g of 2.5M sodium hydroxide solution was added. The collected crude product was concentrated to obtain 550 g of gel-like functionalized macromolecular intermediates with a viscosity of 3000 cps. The intermediate 2 is kept for use.
Example Embodiment
[0042] Example 3
[0043]
[0044] In a 2L reaction flask, add sodium 2-acrylamide-2-methylpropanesulfonate (20.0g), potassium persulfate (12.0g) and water, mix and stir until potassium persulfate is completely dissolved, and add it to the functionalization in Application Example 2. The macromolecular intermediate (400g) was stirred evenly to obtain the macromonomer solution, which was placed for later use. Add butyl acetate (2.5L) and the ethyl acetate solution (35g) of 10% butyl acetate cellulose to the 5L reaction kettle, blow in nitrogen, increase the temperature of the system to 63°C, add the above macromonomer solution and four Methyl ethylenediamine (20 mL), then the reaction was stirred at 58°C for 3 hours. After the reaction, the reaction mixture was washed sequentially with butyl acetate and acetone, filtered with suction, and dried under vacuum to obtain polyvinyl alcohol embolic microspheres 3 (80 g).
[0045] After being swelled and sieved, the embolic microspheres a...
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