| 含全氟壬烯基的丙烯酸酯的合成 |
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| 引用本文： | 史鸿鑫,裘飞,项菊萍,武宏科,陈立军.含全氟壬烯基的丙烯酸酯的合成[J].精细化工,2010,27(2). |
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| 作者姓名： | 史鸿鑫 裘飞 项菊萍 武宏科 陈立军 |
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| 作者单位： | 浙江工业大学,绿色化学合成技术国家重点实验室培育基地,浙江,杭州,310032 |
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| 基金项目： | 浙江省自然科学基金资助项目(Y405396)~~ |
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| 摘 要： | 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%。
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| 关 键 词： | 含氟丙烯酸酯 羟甲基化 酯化 全氟壬烯 |
Synthesis of a Acrylate Containing Perfluorononenyl |
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| SHI Hong-xin,QIU Fei,XIANG Ju-ping,WU Hong-ke,CHEN Li-jun.Synthesis of a Acrylate Containing Perfluorononenyl[J].Fine Chemicals,2010,27(2). |
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| Authors: | SHI Hong-xin QIU Fei XIANG Ju-ping WU Hong-ke CHEN Li-jun |
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| Affiliation: | Zhejiang University of Technology/a>;State Key Laboratory Breeding Base of Green Chemistry Synthesis-Technology/a>;Hangzhou 310032/a>;Zhejiang/a>;China |
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| Abstract: | p-Perfluorononenoxy benzamide(Ⅰ) reacted with formaldehyde,then was esterified with acrylic acid to produce p-perfluorononenoxybenzamidomethyl acrylate(Ⅱ).This product was characterized by IR,1HNMR,~(19)FNMR.Ⅰ reacted with formaldehyden(Ⅰ): n(HCHO)=1: 6.0] at 70 ℃ for 8 h in the presence of sodium carbonate to give N-hydroxymethyl-p-perfluorononenoxy-benzamide(Ⅲ) in the yield of 84.7%.Ⅲ reacted with acrylic acid in toluene,n(Ⅲ): n(CH_2-CHCOOH-)=1: 2.0,catalyzed by toluene p-sulfonic acid,and refluxed for 8 h to give Ⅱ in the yield of 74.2%. |
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| Keywords: | fluorinated acrylate hydroxymethylation esterification perfluorous nonene |
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