Cyclic carbonate monomer containing nitric oxide donor and its preparation and application
A technology for cyclic carbonates and monomers, applied in the field of cyclic carbonate monomers, polymers and their preparation, can solve the problems of complex preparation process, poor controllability, and low loading capacity, and achieve simple preparation, simple synthesis, The effect of high NO load
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Embodiment 1
[0057] The synthesis of nitrate trimethylolethane cyclocarbonate monomer (NEC) is as follows:
[0058]
[0059] Compound 1 (10 g, 54.64 mmol) was dissolved in 100 mL of acetonitrile, silver nitrate (27.84 g, 0.16 mol) was added, and reacted overnight at 70°C. After the reaction finished, the reaction solution was filtered, and the filtrate was washed with 150mL dichloromethane (CH 2 Cl 2 ) was diluted, extracted three times with water, the organic phase was dried with anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain yellow oily compound 2, yield: 86.3%.
[0060] Under nitrogen protection, compound 2 (7 g, 42.39 mmol) was dissolved in dried THF (150 mL), then cooled to 0 °C, ethyl chloroformate (9.2 g, 84.77 mmol) was added, and then Et 3 N (9.87g, 97.49mmol). After the dropwise addition was completed, the system continued to react overnight at room temperature. After the reaction, filter out the produced Et 3 N·HCl, the filtrate was...
Embodiment 2
[0063] The synthesis of nitrate trimethylolpropane cyclocarbonate monomer (NPC) is as follows:
[0064]
[0065] Compound 4 (10 g, 50.74 mmol) was dissolved in 100 mL of acetonitrile, silver nitrate (25.35 g, 0.15 mol) was added, and reacted overnight at 70°C. After the reaction finished, the reaction solution was filtered, and the filtrate was washed with 150mL dichloromethane (CH 2 Cl 2 ) was diluted, extracted three times with water, the organic phase was dried with anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain yellow oily compound 5, yield: 88.6%.
[0066] Under nitrogen protection, compound 5 (7 g, 39.07 mmol) was dissolved in dried THF (150 mL), then cooled to 0 °C, ethyl chloroformate (8.48 g, 78.14 mmol) was added, and then Et was added dropwise. 3 N (9.09 g, 89.86 mmol). After the dropwise addition was completed, the system continued to react overnight at room temperature. After the reaction, filter out the produced Et 3...
Embodiment 3
[0069] Ring-opening copolymerization of nitrate trimethylolethane cyclocarbonate monomer, the process is as follows:
[0070]
[0071] The ring-opening copolymerization of nitrate trimethylolethane cyclocarbonate monomer is based on polyethylene glycol (Mn 5000) as an initiator, dichloromethane as a solvent, and bis(bistrimethylsilyl)amine zinc as a catalyst , carried out at 40 °C. The reaction was fed in a glove box, using a one-pot method, and reacted for 24 hours. After the reaction, the polymer was finally purified by precipitation with ether. The copolymer composition and GPC characterization are shown in Table 1.
[0072] Table 1. Ring-opening copolymerization of nitrate trimethylolethane cyclocarbonate monomer
[0073]
[0074] (a). The mass percent of nitrate trimethylolethane cyclocarbonate monomer when feeding
[0075] (b). The mass percent of nitrate trimethylolethane cyclocarbonate monomer on the polymer chain
[0076] Synthesis of polymer PEG-PNTC (8.1k...
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