Ph-reducing double-responsive polymer embolic agent for catheter-free embolization of tumors and its synthesis
An embolic agent and polymer technology, which is applied in the field of polymer embolizing agent for catheterless embolization of tumors with pH-reduction dual response and its synthesis, and can solve the problems of intraductal gelation and the like
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Embodiment 1
[0052] Add 1g of newly prepared L-threonine NCA to a 50mL three-necked flask, dissolve in 3mL redistilled 1,4-dioxane, and 2 Add 2.835 mg of piperazine under protective conditions to carry out the polymerization reaction. After the polymerization reaction is completed, add ethanol to obtain a white precipitate, centrifuge, and wash the white precipitate with ethanol and ether for 2 to 3 times, and dry it in vacuum at 40°C for 24 hours. White poly (L-threonine) (PLGThr) was obtained. Add 0.4 g of PLGThr to a 50 mL three-necked flask, suspend it in 2 mL of 1,4-dioxane, and 2 Added newly prepared L-glutamic acid-5-benzyl ester-NCA (BLG-NCA) and L-cysteine NCA (LCys-NCA) under protective conditions, reacted for 72 hours, and precipitated with absolute ethanol to obtain a white solid as poly (L-glutamic acid-5-benzyl ester-L-cysteine)-poly(L-threonine)-poly(L-glutamic acid-5-benzyl ester-L-cysteine)( P(BLG-LCys)-PLGThr-P(BLG-LCys)), filtered, and then added to a round-bottomed ...
Embodiment 2
[0060] Add 0.8g of fresh L-threonine NCA to a 50mL three-necked flask, dissolve it with 3mL redistilled 1,4-dioxane, and 2 Add 0.42 mL of 1,4-cyclohexanediamine in 1,4-dioxane solution with a mass volume concentration of 5.4 mg / mL under protective conditions, react at room temperature for 48 hours, add ethanol to obtain a white precipitate, centrifuge, wash with ethanol, ether After washing 2-3 times, vacuum drying at 40°C for 24 h, the white poly(L-threonine) (PLGTHr) was obtained; 0.4 g of PLGThr was added to a 50 mL three-necked flask, and suspended in 2 mL of 1, 4-dioxane, in N 2 Add 0.35g of fresh L-glutamic acid-5-benzyl ester-NCA (BLG-NCA) and 0.28g of L-tyrosine NCA (LTyr-NCA) under protective conditions, react at 35°C for 48 h, and use anhydrous Ethanol precipitation, the solid white obtained is poly(L-glutamic acid-5-benzyl ester-L-tyrosine)-poly(L-threonine)-poly(L-glutamic acid-5-benzyl ester- L-Tyrosine) (P(BLG-LTyr)-PLGThr-P(BLG-LTyr)), filtered, and then added...
Embodiment 3
[0065] Add 2mL of triethylamine and 1,4-dioxane mixed solution in 50mL three-necked flask, the volume ratio of triethylamine and 1,4-dioxane in this mixed solution is 25: 1, in N 2 Add 0.35g of newly prepared L-glutamic acid-5-benzyl ester-NCA (BLG-NCA) and 0.20g of L-cysteine NCA (LCys-NCA) under protective conditions, react at 35°C for 48 h, and use Precipitate with water and ethanol, the obtained white solid is poly(L-glutamic acid-5-benzyl ester-L-cysteine) [P(BLG-LCys)], wash with ethanol and ether three times respectively, and CIA at 40°C Vacuum dried for 24h. Add 0.5g of P(BLG-LCys) into a 50 mL three-neck flask filled with 5 mL of DMF, dissolve it, and 2 Add 0.25g polyethylene glycol 1000 and 2mL hydrogen bromide aqueous solution under protective conditions, and reflux at 80°C for 8h; add hydrochloric acid aqueous solution with a pH value of 2 to obtain a large amount of white precipitate, filter, and then add 30 mL of the mixed solution to the round bottom In the ...
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