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以p-全氟壬烯氧基苯甲酰氯(Ⅰ)和芝麻酚(Ⅱ)为原料,经酯化反应,制备p-全氟壬烯氧基苯甲酸-3,4-亚甲二氧基苯基酯(Ⅲ),用FTIR、1HNMR、19FNMR对其结构进行了表征。考察了缚酸剂、反应温度、反应时间、原料配比对酯化反应收率的影响。优化了酯化反应工艺,得到合成p-全氟壬烯氧基苯甲酸-3,4-亚甲二氧基苯基酯较佳的工艺条件为:二甲基甲酰胺(DMF)为溶剂,三乙胺(NEt3)为缚酸剂,n(Ⅰ)∶n(Ⅱ)∶n(NEt3)=1∶2∶1,-5℃反应4 h,在该条件下收率达79.0%。
Using p-perfluoro-nonenoxybenzoyl chloride (Ⅰ) and sesamol (Ⅱ) as starting materials, p-perfluorononinyloxybenzoic acid-3,4-methylenedioxy Its structure was characterized by FTIR, 1HNMR and 19F NMR. The effects of acid-binding agent, reaction temperature, reaction time and raw material ratio on the yield of esterification reaction were investigated. Optimization of the esterification reaction process, the synthesis of p-perfluoro-nonenoxybenzoic acid -3,4-methylenedioxyphenyl ester preferred process conditions: dimethylformamide (DMF) as a solvent, The yield of NEt3 was 79.0% under the conditions of 4 hours reaction at -5 ℃, with n (Ⅰ): n (Ⅱ): n (NEt3) = 1: 2.