含全氟环丁基芳基醚结构硅氧烷单体的合成与表征

Synthesis and Characterization of Siloxane Monomer Containing Perfluorocyclobutyl Aryl Ether Groups

以4-溴苯酚为原料,通过O-烷基化反应合成中间体1-溴-4-(2-溴-1,1,2,2-四氟乙氧基)苯,然后通过脱卤反应合成中间体1-溴-((1,2,2-三氟乙烯基)氧基)苯,再通过格氏反应合成中间体乙氧基二甲基(4-((1,2,2-三氟乙烯基)氧基)苯基)硅烷,最后通过环化反应合成含全氟环丁基芳基醚结构的硅氧烷单体。通过傅里叶变换红外光谱(FT-IR)、核磁共振(NMR)对各中间体和单体的结构进行了表征。结果表明,含全氟环丁基芳基醚结构硅氧烷单体成功合成。

1-Bromo-4-(2-bromo-1,1,2,2-tetrafluoroethoxy)benzene was synthesized by O-alkylation reaction using 4-bromophenol as a raw material,and then 1-bromo-((1,2,2-trifluoroethenyl)oxy)benzene was prepared by dehalogenation reaction,followed by synthesis of ethoxydimethyl(4-((1,2,2-trifluoroethenyl)oxy)phenyl)silane by Grignard reaction,and finally the siloxane monomers containing perfluorocyclobutyl aryl ether structure were obtained by cyclization dimerization.The structures of each intermediate and monomer were characterized by Fourier transform infrared spectroscopy(FT-IR)and nuclear magnetic resonance(NMR).The results showed that the siloxane monomer containing perfluorocyclobutyl aryl ether structures was successfully synthesized.