Y-type drug delivery material with pH responsiveness and preparation method thereof
A responsive, drug-based technology, applied in the field of pH-responsive Y-type polymer drug delivery materials and its preparation, can solve the problems of cumbersome synthesis and poor biocompatibility of polymer drug delivery materials, and achieve good biocompatibility Effect
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Embodiment 1
[0035] 1) Add 2,2-dimethylolpropionic acid (100mmol), 2,2-dimethoxypropane (110mmol) and 50mL acetone sequentially into a 250ml single-necked bottle, start stirring, and add p-toluenesulfonic acid (8mmol), after reacting at room temperature for 5 hours, sodium acetate (10mmol) was added to terminate the reaction, filtered, and the filtrate was spin-dried to obtain compound II.
[0036]
[0037] 2) Add polyethylene glycol monomethyl ether (average number average molecular weight is 1000, 4mmol), 4-N, N'-dimethylaminopyridine (8mmol), dicyclohexyl carbon to a dry 100ml three-necked flask successively Diimine (12mmol) and 50mL dry dichloromethane solution, under the protection of nitrogen, dropwise add the mixed solution of compound II (12mmol) and dichloromethane (15mL), after stirring for 48 hours, filter, the concentrated solution was precipitated in ether Polymer III-1 was obtained.
[0038]
[0039] In the formula, n=22 or 44
[0040] 3) Add polymer III-1 (2 mmol) an...
Embodiment 2
[0048] 1) with embodiment 1 step 1)
[0049] 2) with embodiment 1 step 2)
[0050] 3) with embodiment 1 step 3)
[0051] 4) with embodiment 1 step 4)
[0052] 5) Under the protection of an inert gas, polymer V-1 (0.1mmol), copper bromide (0.01mmol), cuprous bromide (0.2mmol), pentamethylene divinyltriamine (0.2mmol) and 2, 2'-Dimethyl-1,3-dioxolane acrylate (8mmol) in toluene (2mL) mixed solution was reacted at 60°C under nitrogen protection for 6 hours, the reaction system was aired, diluted with 40mL tetrahydrofuran, and the The copper ions were removed by neutral alumina column chromatography, the eluent was collected and concentrated, and the product I-2 was obtained by precipitating in diethyl ether / n-hexane (v / v=1:5) precipitant.
Embodiment 3
[0054] 1) with embodiment 1 step 1)
[0055] 2) with embodiment 1 step 2)
[0056] 3) with embodiment 1 step 3)
[0057] 4) with embodiment 1 step 4)
[0058] 5) Under the protection of an inert gas, polymer V-1 (0.1mmol), copper bromide (0.01mmol), cuprous bromide (0.2mmol), pentamethylene divinyltriamine (0.2mmol) and 2, 2'-Dimethyl-1,3-dioxolane acrylate (8mmol) in toluene (2mL) mixed solution was reacted at 60°C under nitrogen protection for 4 hours, the reaction system was aired, diluted with 40mL tetrahydrofuran, and the The copper ions were removed by neutral alumina column chromatography, the eluent was collected and concentrated, and the product I-3 was obtained by precipitating in diethyl ether / n-hexane (v / v=1:5) precipitant.
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