A kind of amphiphilic glycoside functionalized hyperbranched ferrocene and preparation method thereof
A ferrocene and functionalization technology, applied in the field of metallocene polymer materials, can solve the problems of poor hydrophilicity and poor biological response, achieve good amphiphilicity, avoid the use of toxic catalysts, and overcome hydrophilicity poor effect
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Embodiment 1
[0043]Step (1), add 1.5g (5.5mmol) of 1,1'-ferrocenedicarboxylic acid and 35ml of anhydrous methanol into a 250mL three-neck round bottom flask in turn, add 2.8ml (20mmol) of triethylamine dropwise, and the color of the solution deepens , use an ice-salt bath to lower the reaction temperature, and control it between 0 and 5°C. At this time, 1.5ml (20mmol) of thionyl chloride was slowly added dropwise through a constant pressure dropping funnel. The reaction was violent, and a large amount of white smoke was generated. After completion, the stirring reaction was continued at this temperature for 1 h. Remove the ice-salt bath, heat in an oil bath, raise to 50°C, and react for 4.5 hours. After cooling the reaction solution naturally, take out the three-necked flask, pour the reaction mixture into a 250mL single-necked flask, and install it on a rotary evaporator. Control the temperature of the rotary evaporator to gradually increase from 25°C to 45°C, remove methanol by rotary ev...
Embodiment 2
[0050] Step (1), add 1.5g of 1,1'-ferrocenedicarboxylic acid and 35ml of anhydrous methanol into a 250mL three-necked round bottom flask in sequence, add 2.8ml of triethylamine dropwise, lower the reaction temperature, and control it at 0-5°C In between, 1.5ml of thionyl chloride was slowly added dropwise, stirred for 1h, heated to 45°C, reacted for 5h, cooled the reaction solution naturally, poured the reaction mixture into a 250mL single-necked flask, and removed methanol by rotary evaporation to obtain a sticky substance. Then 40ml of saturated sodium chloride solution was added thereto, extracted with 90mL of ethyl acetate, the organic phases were combined and poured into a separatory funnel, the layers were static, and the upper layer was taken. Then the ethyl acetate was removed by rotary evaporation, and the brown needle-shaped 1,1'-ferrocenedicarboxylate (Formula 1-1) was obtained by drying, with a yield of 87%.
[0051] CH at room temperature 3 OH (26mL) was added dr...
Embodiment 3
[0057] Step (1), add 1.5g of 1,1'-ferrocenedicarboxylic acid and 35ml of anhydrous methanol into a 250mL three-necked round bottom flask in sequence, add 2.8ml of triethylamine dropwise, lower the reaction temperature, and control it at 0-5°C In between, 1.5ml of thionyl chloride was slowly added dropwise, stirred for 1h, heated to 55°C, reacted for 4h, cooled the reaction solution naturally, poured the reaction mixture into a 250mL single-necked flask, and removed methanol by rotary evaporation to obtain a sticky substance. Then 40ml of saturated sodium chloride solution was added thereto, extracted with 90mL of ethyl acetate, the organic phases were combined and poured into a separatory funnel, the layers were static, and the upper layer was taken. Then the ethyl acetate was removed by rotary evaporation, and the brown needle-shaped 1,1'-ferrocenedicarboxylate (Formula 1-1) was obtained by drying, with a yield of 80.1%.
[0058] CH at room temperature 3 OH (26mL) was added ...
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