A kind of multi-block polyethylene glycol containing hydroxyl group and active double bond and preparation method thereof
A technology of polyethylene glycol and polyethylene glycol diacrylate, which is applied in the field of polymer preparation, can solve the problems of few surface groups, inability to achieve better loading capacity, etc., and achieves good stability and small immunogenicity. and antigenicity and low toxicity
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Embodiment 1
[0035] 10g (0.025mol) polyethylene glycol diacrylate (Mn=400), 5g (0.025mol) glutaraldehyde 50% aqueous solution, 0.28g (0.0025mol) 1,4-diazide bicyclo [2.2.2] octane Alkane (DABCO) catalyst, 0.014g p-hydroxyphenol polymerization inhibitor, 50mL acetone as solvent, after heating to reflux for 96 hours, distill off the solvent under reduced pressure, add dichloromethane, and dry with anhydrous magnesium sulfate for 24 hours, filter, and the filtrate passes through Dichloromethane was distilled off under reduced pressure, and the crude product was precipitated with ether to obtain multi-block polyethylene glycol containing hydroxyl groups and active double bonds. Mn(GPC)=4500, PDI(GPC)=1.8
Embodiment 2
[0037] 10g (0.01) polyethylene glycol diacrylate (Mn=1000), 2g (0.01mol) glutaraldehyde 50% aqueous solution, 0.12g (0.001mol) 1,4-diazide bicyclo [2.2.2] octane (DABCO) catalyst, 0.01g p-hydroxyphenol polymerization inhibitor, 50mL acetone as solvent, after heating and refluxing for 96 hours, the solvent was distilled off under reduced pressure, dichloromethane was added, and when drying with anhydrous magnesium sulfate for 24 hours, filter, and the filtrate was passed through Dichloromethane was distilled off under high pressure, and the crude product was precipitated with ether to obtain multi-block polyethylene glycol containing hydroxyl groups and active double bonds. Mn(GPC)=7200, PDI(GPC)=2.0
[0038]
Embodiment 3
[0040] 10g (0.025mol) polyethylene glycol diacrylate (Mn=400), 3.35g (0.025mol) terephthalaldehyde, 0.28g (0.0025mol) 1,4-diazidebicyclo[2.2.2]octane (DABCO) catalyst, 0.014g p-hydroxyphenol polymerization inhibitor, 50mL acetone as solvent, after heating and refluxing for 96 hours, the solvent was distilled off under reduced pressure, dichloromethane was added, and when drying with anhydrous magnesium sulfate for 24 hours, filter, and the filtrate was filtered by reducing Dichloromethane was distilled off under high pressure, and the crude product was precipitated with ether to obtain multi-block polyethylene glycol containing hydroxyl groups and active double bonds. Mn(GPC)=5300, PDI(GPC)=1.8
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