Six-arm thermosensitive polymer and preparation method thereof
A temperature-sensitive polymer and temperature-sensitive monomer technology, applied in the fields of polymer chemistry and material chemistry, can solve problems such as difficulty in control, affecting polymer properties and scope of use, and runaway functionality at the end of the chain structure. Good effect for allergy
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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 dipentaerythritol, an acid-binding agent, a catalyst and an acylating agent having a structure of formula (II) in a solvent to obtain an initiator having a structure of formula (III);
[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-...
Embodiment 1
[0072]Add dipentaerythritol (2.55g, 10mmol) into a solution containing triethylamine (6.19g, 61mmol) and 50ml of dichloromethane, and stir for 30min under ice-bath conditions. 2-Bromoisobutyryl bromide (14.07 g, 61 mmol) was added slowly over 1 hour through a constant pressure dropping funnel, 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 12 hours. After the reaction, the obtained product was washed successively with 5% sodium bicarbonate solution (100ml*3), saturated saline (100ml*3), and deionized water (100ml*3). The washed organic layer was rotary evaporated to remove the solvent, dissolved in dichloromethane, slowly added dropwise into glacial ether, and left standing at 0°C for 12 hours. Filter through a funnel and wash with cold diethyl ether (10ml). At room temperature, dry in a vacuum oven to obtain a white crystal initiator. figure 1 The initiator prepared for thi...
Embodiment 2
[0078] Dipentaerythritol (2.55g, 10mmol) was added to a solution containing pyridine (5.135g, 65mmol) and 100ml of tetrahydrofuran, and stirred for 30min under ice-bath conditions. 2-Bromoisobutyryl bromide (14.95 g, 65 mmol) was slowly added through a constant pressure dropping funnel over 1 hour, and 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, the obtained product was washed successively with 5% sodium bicarbonate solution (100ml*3), saturated saline (100ml*3), and deionized water (100ml*3). The washed organic layer was rotary evaporated to remove the solvent, dissolved in dichloromethane, slowly added dropwise into glacial ether, and left standing at 0°C for 12 hours. Filter through a funnel and wash with cold diethyl ether (10ml). At room temperature, dry in a vacuum oven to obtain a white crystal initiator.
[0079] Add 1 g of N-isopropylacrylamide, 0.3363 g of...
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