Adamantyl four-arm temperature sensitive polymers and a preparing method thereof
A temperature-sensitive polymer and temperature-sensitive monomer technology, which is applied in the fields of polymer chemistry and material chemistry, can solve problems that affect the performance and application range of polymers, are difficult to control, and the terminal functionality of the chain structure is out of control.
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[0042] The present application also provides a preparation method of the above-mentioned thermosensitive polymer, comprising the following steps:
[0043] A), under inert gas and anhydrous conditions, react 1,3,5,7-tetrahydroxyadamantane, acid-binding agent, catalyst with an acylating agent having a structure of formula (II) in a solvent to obtain (Ⅲ) Initiator of structure;
[0044] B), under the protection of an inert gas, react the initiator, temperature-sensitive monomer, catalyst and complexing agent in a solvent to obtain an active temperature-sensitive polymer with a structure of formula (IV); the temperature-sensitive The neutral monomer is selected from N-isopropylacrylamide, N-propylacrylamide, N-cyclopropylacrylamide, N,N-diethylacrylamide, N-vinylisopropanamide, N-vinyl N-propionamide, N-vinylcaprolactam, N-vinylpyrrolidone, N-acryloylpyrrolidine, N-acryloyl-N'-n-propiperazine, N-(2,2-dimethyl-1,3 One or more of -dioxan-5 alcohol)-acrylamide and N-(2-ethoxy-1,3-d...
Embodiment 1
[0072] 1,3,5,7-Tetrahydroxyadamantane (1.00g, 5mmol) was added to a solution containing pyridine (1.678g, 21.25mmol) and 10ml of acetonitrile, stirred for 30min under ice-bath conditions, and 2-bromoisobutyl Acyl bromide (4.89g, 21.25mmol) was added slowly within 1 hour through a constant pressure dropping funnel, kept at a low temperature for 1 to 2 hours, then gradually rose to room temperature, and continued to react for 12 hours; Sodium hydrogen solution (100ml*3), saturated brine (100ml*3), and deionized water (100ml*3) were washed sequentially, and the washed solution was removed by rotary evaporation. After the crude product was dissolved in ethyl acetate, the Ethyl acetate: n-hexane 1:2 (V / V) was used as the eluent to pass through a neutral alumina column, and the solvent was removed by rotary evaporation, and dried in a vacuum oven at 40°C to obtain white crystals. figure 1 Tetrakis-(2-bromoisobutyryl)adamantane initiator prepared for this step as the nucleus 1 H-NMR...
Embodiment 2
[0078] 1,3,5,7-Tetrahydroxyadamantane (1.00g, 5mmol) was added to a solution containing triethylamine (2.277g, 22.5mmol) and 10ml, and stirred for 30min under ice-bath conditions. 2-Bromoisobutyryl bromide (5.175 g, 22.5 mmol) was slowly added through a constant pressure dropping funnel over 1 hour, and the temperature was kept at low temperature for 1-2 hours. Then it was gradually raised to room temperature, and the reaction was continued for 24 hours. After the reaction, wash with 5% sodium bicarbonate solution (100ml*3), saturated saline (100ml*3), and deionized water (100ml*3) in sequence. The washed solution was evaporated to remove the solvent, the crude product was dissolved in ethyl acetate, and passed through a neutral alumina column with ethyl acetate:n-hexane 1:2 (V / V) as the eluent. The solvent was removed by rotary evaporation, and dried in a vacuum oven at 40°C to obtain a white crystal initiator.
[0079] Add 4 g of N-isopropylacrylamide, 0.07 g of an initiat...
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