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p-全氟壬烯氧基苯甲酸芝麻酚酯的合成
引用本文:史鸿鑫,吴健,武宏科,陈立军,赵丽君.p-全氟壬烯氧基苯甲酸芝麻酚酯的合成[J].精细化工,2012,29(8):734-737.
作者姓名:史鸿鑫  吴健  武宏科  陈立军  赵丽君
作者单位:浙江工业大学化学工程与材料科学学院绿色化学合成技术国家重点实验室培育基地,浙江杭州,310032
基金项目:浙江省科技厅创新团队资助项目 2011R09002-10
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%。

关 键 词:含氟苯甲酸芝麻酚酯  酯化反应  缚酸剂  表征  表面活性剂
收稿时间:2012/2/15 0:00:00
修稿时间:5/2/2012 12:00:00 AM

Synthesis of Sesamol p-perfluorononenebenzonate
SHI Hong-xin , WU Jian , WU Hong-ke , CHEN Li-jun , ZHAO Li-jun.Synthesis of Sesamol p-perfluorononenebenzonate[J].Fine Chemicals,2012,29(8):734-737.
Authors:SHI Hong-xin  WU Jian  WU Hong-ke  CHEN Li-jun  ZHAO Li-jun
Affiliation:Zhejiang University of Technology,Zhejiang University of Technology,Zhejiang University of Technology,Zhejiang University of Technology
Abstract:3,4-Methylenedioxyphenol p-perfluorononenebenzonate(Ⅲ) was synthesized by esterification from p-perfluorononenebenzoyl chloride(Ⅰ) and 3,4-methylenedioxy-phenol(Ⅱ).The product was characterized by means of FTIR,1HNMR,19FNMR.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 ascertained as follows:n(Ⅰ)∶ n(Ⅱ)∶ n(triethylamine)=1∶ 2∶ 1,and the reactants were agitated in DMF at-5 ℃ for 4 h to give 3,4-methylenedioxyphenol p-perfluorononenebenzonate in the yield of 79.0%.
Keywords:Fluorine-containing sesamol benzoate  esterofocation  catalyst  characterization
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