Noda Takumi, Tanaka Anri, Akae Yosuke, Kohsaka Yasuhiro
Faculty of Textile Science and Technology, Shinshu University 3-15-1 Tokida Ueda Nagano 386-8657 Japan.
Japan Society for the Promotion of Science (JSPS) Tokyo Japan.
RSC Adv. 2023 Jul 7;13(29):20336-20341. doi: 10.1039/d3ra03461e. eCollection 2023 Jun 29.
Main-chain scission of polymers induces a significant decrease in molecular weight and accompanying changes in physical properties and is important for applications in materials engineering, such as in photoresists and adhesive dismantling. In this study, we focused on methacrylates substituted with carbamate groups at the allylic positions for the purpose of developing a mechanism that efficiently cleaves the main chain in response to chemical stimuli. Dimethacrylates substituted with hydroxy groups at the allylic positions were synthesized by the Morita-Baylis-Hillman reaction of diacrylates and aldehydes. The polyaddition with diisocyanates afforded a series of poly(conjugated ester-urethane)s. These polymers underwent a conjugate substitution reaction with diethylamine or acetate anion at 25 °C, resulting in main-chain scission accompanied by decarboxylation. A side reaction by the re-attack of the liberated amine end to the methacrylate skeleton proceeded, whereas it was suppressed for the polymers with an allylic substitute of the phenyl group. Therefore, the methacrylate skeleton substituted with phenyl and carbamate groups at the allylic position is an excellent decomposition point that induces selective and quantitative main-chain scission with weak nucleophiles, such as carboxylate anions.
聚合物的主链断裂会导致分子量显著降低,并伴随物理性质的变化,这对于材料工程中的应用非常重要,例如在光刻胶和粘合剂拆解方面。在本研究中,我们聚焦于在烯丙基位置被氨基甲酸酯基团取代的甲基丙烯酸酯,目的是开发一种能响应化学刺激而有效裂解主链的机制。通过二丙烯酸酯与醛的森田 - 贝利斯 - 希尔曼反应合成了在烯丙基位置被羟基取代的二甲基丙烯酸酯。与二异氰酸酯的聚加成反应得到了一系列聚(共轭酯 - 聚氨酯)。这些聚合物在25℃下与二乙胺或乙酸根阴离子发生共轭取代反应,导致主链断裂并伴随脱羧反应。释放出的胺端重新进攻甲基丙烯酸酯骨架会发生副反应,而对于在烯丙基位置有苯基取代基的聚合物,这种副反应受到抑制。因此,在烯丙基位置被苯基和氨基甲酸酯基团取代的甲基丙烯酸酯骨架是一个优异的分解位点,能在诸如羧酸根阴离子等弱亲核试剂作用下引发选择性和定量的主链断裂。