Temperature-sensing amphiphilic polyether dendrons and their preparation method and use
A branching and amphiphilic technology, applied in the chemical field, can solve the problems of no micelle-coated podophyllotoxin reported in the literature, and achieve the effects of shortening the synthesis cycle, prolonging the reaction time, and mild preparation conditions
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Embodiment 1
[0045] Add 1.21g of the second-generation polyether dendron at the end of the ester center and 50mL of tetrahydrofuran into a dry round-bottomed flask. After stirring and dissolving, add 0.10g of lithium aluminum hydride under stirring in an ice-water bath, and react at room temperature for 20 hours. Add 30mL of 5% sodium hydroxide solution, filter, distill off the solvent, dissolve the residue with dichloromethane, wash the organic phase with saturated sodium chloride solution, dry, filter, and distill off the solvent to obtain the second Generation of polyether dendrons (G2-CH 2 OH), yield 80.5%.
[0046] Add 3.88g compound G2-CH successively in the dry two-necked flask 2 OH, 4.5mL dimethylformamide and 50mL dichloromethane, add dropwise a dichloromethane solution of thionyl chloride (prepared by dissolving 0.92g thionyl chloride in 30mL dichloromethane) under stirring, and dropwise, After reacting at room temperature for 2 hours, the organic phase was washed three times w...
Embodiment 2
[0049] Add 1.66g G3-COOMe and 50mL tetrahydrofuran into a dry round bottom flask, stir to dissolve, add 0.09g lithium aluminum hydride under stirring in an ice-water bath, react at room temperature for 24 hours, add 30mL 5% sodium hydroxide solution, filter , evaporate the solvent, and dissolve the residue with dichloromethane, wash the organic phase with saturated sodium chloride solution, dry, filter, and evaporate the solvent to obtain the third-generation polyether branching base of the methylol center terminal group (G3- CH 2 OH), yield 81.1%.
[0050] In the dry two-necked flask, add 3.93g compound G3-CH successively 2 OH, 4.5mL dimethylformamide and 50mL dichloromethane, add thionyl chloride dropwise under stirring 2 Cl 2 Solution (prepared by dissolving 0.31g of thionyl chloride in 30mL of dichloromethane), after dropping, reacted at room temperature for 4h, washed the organic phase three times with 150mL of saturated sodium bicarbonate solution, dried, filtered, an...
Embodiment 3
[0053] Weigh 50 mg of the third-generation temperature-sensitive amphiphilic polyether dendron (G3-COOMe) and dissolve it in 10 mL of THF. After it is completely dissolved, slowly add 10 mL of distilled water to the solution while stirring, and evaporate the organic solvent at room temperature. , the residual solution was transferred to a 25mL volumetric flask to obtain a 2.0mg / mL micellar solution. Use a pipette to pipette different volumes of micellar solution into several 10mL volumetric flasks, and then add 1.2×10 -4 mg / mL pyrene solution in acetone 50 μL, evaporate the acetone at room temperature, dilute to the mark with distilled water. The resulting solution was sonicated for 30 min, left at room temperature for 24 h, and the critical micelle concentration (CMC) of G3-COOMe measured by fluorescence spectroscopy was 7.7×10 -6 M, this result is consistent with the CMC of the polymer (generally ~ 10 -6 M) are equivalent, indicating that G3-COOMe self-assembled into stabl...
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