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Polymers synthesis Polymerization under oil bath heating in RTIL as a reaction medium The PAs were prepared by the following general procedure: as an example for the preparation of PA5cI, 0.100 g (0.244 mmol) of diacid 1 and 0.061 g (0.244 mmol) of diamine 2c were dissolved in 0.150 g of 1,3-diisopropylimidazolium bromide (1,3-(isopr)2im]Br), then 0.13 mL (0.488 mmol) of TPP was added. The whole solution was heated at 110 C for 2.5 h. The solution becomes more viscous by progress of the polymerization reaction. The resulting product was dissolved in 1 mL of DMF and was poured into a beaker containing 30 mL of methanol (ethanol), or methanol (ethanol) was directly added to the reaction vessel without using DMF. The obtained solid was filtered off and dried under vacuum to give 0.146 g (94%) of PA5cI. Polymerization under oil bath heating in NMP as a reaction medium The PAs were prepared by the following general procedure. Taking PA5cII as an example, a mixture of 0.06 g (0.244 mmol) of diamine 2c, 0.10 g (0.244 mmol) of diacid 1, 0.060 g of CaCl2, 0.15 mL of pyridine, 0.14 mL of TPP, and 0.5 mL of NMP was placed into the flask equipped with a mechanical stirrer and a condenser. The mixture blanketed by nitrogen was stirred and refluxed for 5 h. At the end of the reaction, the obtained polymer solution was trickled into 20 mL of stirred methanol or ethanol. The white-stringy polymer was washed thoroughly with hot water and methanol, collected by filtration and dried at 100 C under reduced pressure to give 0.138 g (82%) of PA5cII. |
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jiangguofeng
金虫 (著名写手)
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- 专业: 合成药物化学
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聚合物的合成 在反应介质RTIL中油浴加热进行聚合反应，通过下列一般方法制备PA：作为PA5cI制备实例, 0.100 g ( 0.244 mmol)的二酸1和0.061 g ( 0.244 mmol)的二胺2c溶于0.150 g 溴化1,3 -二异丙基咪唑溴( 1,3 - ( isopr) 2im] Br),然后将0.13 mL ( 0.488 mmol)的TPP加进。全部溶液加热110℃2.5小时。由于聚合反应的发展溶液变得更为黏稠。生成的产物溶于1 mL的二甲基甲酰胺中然后倾入装有30 mL甲醇（乙醇)的烧杯中,或者将甲醇（乙醇）直接加到没使用二甲基甲酰胺的反应容器中。滤出得到的固形物然后真空干燥，得到0.146 g (94%)的PA5cI。 在反应介质NMP中油浴加热进行聚合反应，通过下列一般方法制备PA：作为PA5cII制备实例, 0.06 g ( 0.244 mmol)二胺2c、0.10 g ( 0.244 mmol)二酸1、0.060 g的CaCl2、0.15 mL吡啶、0.14 mL的TPP和0.5 mL的NMP组成的混合物投入配有机械搅拌器和冷凝器的烧瓶中。氮气保护下混合物搅拌并回流５小时。 反应结束时，将得到的聚合物溶液一滴滴注入搅拌下的20 mL甲醇或者乙醇中。这种白色粘稠的聚合物用热水和甲醇彻底地洗涤,过滤收集，减压下在100℃干燥，得到0.138 g ( 82%)的PA5cII。 |
2楼2015-04-08 09:36:26
