p-全氟壬烯氧基苯甲酸芝麻酚酯的合成

Synthesis of Sesamol p-perfluorononenebenzonate

摘要:

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FT-IR、1HNMR、13FNMR对其结构进行了表征。考察了催化剂，反应温度和反应时间，原料配比对酯化反应收率的影响。优化了酯化反应工艺，合成p-全氟壬烯氧基苯甲酸-3,4-亚甲二氧基苯基酯较佳工艺条件为：n(I)：n(II)：n(NEt3)=1：2.0 ：1，DMF为溶剂，三乙胺为催化剂， -5℃反应时间4 h，收率79.0％。

Abstract:

3,4-Methylenedioxyphenol p-perfluorononenebenzonate was synthesized by esterification from p-perfluorononenebenzoyl chloride(PFNBC) and 3,4- methylenedioxy- phenol. The product was characterized by FT-IR、1H NMR、13F NMR. The effects of catalyst, reaction temperature, reaction time and the ratio of reactants on the esterification were investigated. The optimum reaction conditions of the esterification were determined as follows: n(PFNBC):n(sesamol):n(NEt3)=1:2.0:1, the reactants were agitate in DMF at -5℃ for 4h to give 3,4-methylenedioxyphenol p-perfluorononenebenzonate in the yield of 79.0 %.