A kind of preparation method of linear polyethylene glycol-dendrimer poly(thioether-amine) block copolymer
A technology of block copolymer and polyethylene glycol monomethyl ether, applied in the field of organic polymers, can solve the problems of high cost, many synthesis steps, long time, etc., and achieve simple steps, clear molecular structure and mild reaction conditions. Effect
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Embodiment example 1
[0024] A linear-dendritic block copolymer was prepared using PEG1000, methacryloyl chloride, mercaptoethylamine, and glycidyl methacrylate as raw materials.
[0025] (1) Preparation of the initiator nucleus G0: Take PEG1000 (20g) and dissolve it in dichloromethane (100mL), wait for it to dissolve completely at 0°C, and use a constant pressure dropping funnel to dissolve methacryloyl chloride ( 2.5 g) was added dropwise to the mixture to react for 24 hours. After the reaction, the resulting product was separated by basic alumina column chromatography, and eluted with dichloromethane as the eluent. The obtained filtrate was concentrated and precipitated in ether for 3 times, and then vacuum-dried overnight to obtain 19 g of white powdery solid.
[0026] (2) Preparation of the 0.5th generation linear-dendritic block copolymer (G0.5): take the G0 product (15g), dissolve it in dimethyl sulfoxide (75mL), and mix mercaptoethylamine with stirring (2.17g) was added to the mixture and ...
Embodiment example 2
[0033] A linear-dendritic block copolymer was prepared using PEG1000, methacrylic anhydride, mercaptoethylamine, and glycidyl methacrylate as raw materials.
[0034](1) Preparation of initiating nucleus G0: Dissolve PEG1000 (20g) in dichloromethane (100mL), wait for it to dissolve completely at room temperature, and use a constant pressure dropping funnel to dissolve methacrylic anhydride (3.7g) under stirring conditions ) was added dropwise in the mixture to react for 24h. After the reaction, the product obtained was separated by basic alumina column chromatography, and dichloromethane was used as the eluent for elution, and the obtained filtrate was concentrated and precipitated in ether for 3 times. It was then vacuum dried overnight to obtain 18 g of a white powdery solid.
[0035] (2) Preparation of the 0.5th generation linear-dendritic block copolymer (G0.5): get the G0 (15g) product, dissolve it in dimethyl sulfoxide (75mL), and mix mercaptoethylamine with stirring (2....
Embodiment example 3
[0042] A linear-dendritic block copolymer was prepared using PEG2000, methacrylic anhydride, mercaptoethylamine, and glycidyl methacrylate as raw materials.
[0043] (1) Preparation of initiating nucleus G0: Take PEG2000 (20g) and dissolve it in 100mL of dichloromethane, and wait for it to dissolve completely at room temperature. Added dropwise to the mixture to react for 24 hours. After the reaction, the resulting product was separated by basic alumina column chromatography and eluted with dichloromethane as the eluent. The obtained filtrate was concentrated and precipitated in ether for 3 times, and then vacuum After drying overnight, 17 g of a white powdery solid was obtained.
[0044] (2) Preparation of the 0.5th generation linear-dendritic block copolymer (G0.5): get the G0 (15g) product, dissolve it in dimethyl sulfoxide (75mL), and mix mercaptoethylamine with stirring (1.12g) was added to the mixture and reacted at room temperature for 2h. After the reaction, the obta...
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