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以p-全氟壬烯氧基苯甲酰胺(Ⅰ)为原料,经羟甲基化和酯化两步反应,制备了p-全氟壬烯氧基苯甲酰胺基丙烯酸甲酯(Ⅱ),用FTIR、1HNMR、19FNMR对其结构进行了表征。中间体N-羟甲基-p-全氟壬烯氧基苯甲酰胺(Ⅲ)的最优合成工艺条件为:n(Ⅰ)∶n(甲醛)=1∶6.0,碳酸钠为碱性催化剂,pH=8.0～10.0,70℃反应8h,Ⅲ的收率84.7%。Ⅱ的最优合成工艺条件为:n(Ⅲ)∶n(丙烯酸)=1∶2.0,甲苯为共沸剂,对甲苯磺酸为催化剂,回流反应8h,Ⅱ的收率74.2%。
The p-perfluorononenoxybenzamido-methyl acrylate (Ⅱ) was prepared from p-perfluorononenoxybenzamide (Ⅰ) by hydroxymethylation and esterification in two steps. Its structure was characterized by FTIR, 1HNMR and 19F NMR. The optimum conditions for the synthesis of the intermediate N-methylol-p-perfluoro-nonenzyloxybenzamide (III) are as follows: n (Ⅰ): n , pH = 8.0 ~ 10.0, reaction at 70 ℃ for 8h, the yield of Ⅲ was 84.7%. The optimal synthesis conditions of Ⅱ were as follows: n (Ⅲ): n (acrylic acid) = 1: 2.0, toluene as entrainer, p - toluene sulfonic acid as catalyst, refluxing for 8h, yield of Ⅱ was 74.2%.