Degradable polyglycol modified ultra-branching polyether ester and preparation method thereof
A polyethylene glycol modification, polyethylene glycol monomethyl ether technology, applied in the field of medical materials, can solve problems such as reduced biocompatibility, and achieve the effect of accelerating the degradation rate
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Embodiment 1
[0022] This embodiment 1 is implemented under the following conditions of implementation and technical requirements:
[0023] a In a four-necked flask equipped with an electromagnetic stirrer, a thermometer, a nitrogen inlet and an addition funnel, first pass nitrogen for 30 minutes to remove the air in the reaction system. 7.096g (0.05mol) boron trifluoride ether BF 3 .OEt 2 And 80ml of dichloromethane was added in the flask, the temperature of the control system was 10°C, within 5 minutes, 11.62g (0.1mol) monomer 3-ethyl-3-butoxetane was slowly added dropwise to the reaction system, maintaining The temperature, the reaction 48h. The reaction solution was slowly added dropwise to excess anhydrous diethyl ether, a white precipitate was produced, filtered, washed, and vacuum-dried at 100°C until constant weight. The productive rate of gained hyperbranched product is 92%, and degree of branching is 0.41 (because 13 C-NMR characterizes the degree of branching of the hyperbran...
Embodiment 2
[0026] This embodiment 2 is implemented under the following conditions of implementation and technical requirements:
[0027] a In a four-necked flask equipped with an electromagnetic stirrer, a thermometer, a nitrogen inlet and an addition funnel, first pass nitrogen for 30 minutes to remove the air in the reaction system. Add 7.096g (0.05mol) of boron trifluoride ether BF3.OEt2 and 80ml of chloroform into the flask, control the temperature of the system at 30°C, and within 5 minutes, 11.62g (0.1mol) of monomer 3-ethyl-3 -Butoxanemethanol was slowly added dropwise into the reaction system, and the temperature was maintained for 24 hours of reaction. The reaction solution was slowly added dropwise to excess anhydrous diethyl ether, a white precipitate was produced, filtered, washed, and vacuum-dried at 100°C until constant weight. The yield of the obtained hyperbranched product was 83.5%, and the degree of branching was 0.47.
[0028] b. After dissolving the product obtained...
Embodiment 3
[0030] This embodiment 3 is implemented under the following conditions of implementation and technical requirements:
[0031] a In a four-necked flask equipped with an electromagnetic stirrer, a thermometer, a nitrogen inlet and an addition funnel, first pass nitrogen for 30 minutes to remove the air in the reaction system. Add 7.096g (0.05mol) boron trifluoride ethyl ether BF3.OEt2 and 80ml xylene into the flask, control the system temperature to 70°C, and within 5 minutes, 11.62g (0.1mol) monomer 3-ethyl-3- Butoxymethanol was slowly added dropwise into the reaction system, and the temperature was maintained for 96 hours of reaction. The reaction solution was slowly added dropwise to excess anhydrous diethyl ether, a white precipitate was produced, filtered, washed, and vacuum-dried at 100°C until constant weight. The yield of the obtained hyperbranched product was 94.5%, and the degree of branching was 0.55.
[0032]b Dissolve the product obtained in a with toluene, react ...
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