Knoevenagel反应合成多氟亚乙基丙二酸酯化合物  

Synthesis of Polyfluoroethylene Malonates by Knoevenagel Reaction

作　　者：王真 吴昊[1] 冯偲[1] 毛俊钧 朱莉丹 洪琼艳 WANG Zhen;WU Hao;FENG Si;MAO Junjun;ZHU Lidan;HONG Qiongyan(School of Materials and Chemical Engineering,Ningbo University of Technology,Ningbo,Zhejiang,315211,China)

机构地区：[1]宁波工程学院材料与化学工程学院,浙江宁波315211

出　　处：《宁波工程学院学报》2020年第3期1-7,共7页Journal of Ningbo University of Technology

基　　金：宁波市自然科学基金(2015A610278);浙江省大学生新苗人才计划(2019R428026);浙江省教育厅(理)/科研计划(Y201533104)。

摘　　要：发展了一种合成多氟亚乙基丙二酸酯化合物的简便通用方法,该方法是基于多氟乙醛半缩醛和丙二酸酯的Knoevenagel反应。发现多氟乙醛半缩醛底物可较为容易地通过多氟乙酸乙酯还原获得,同时考察了碱、酸催化剂、溶剂、催化剂用量等对反应产率的影响。研究结果表明:较优反应条件是摩尔分数均为30%的哌啶和乙酸为催化剂,甲苯为反应溶剂,加热回流24小时。在该条件下,一系列多氟乙醛半缩醛和丙二酸酯可顺利发生Knoevenagel反应,并以中等收率获得多种多氟亚乙基丙二酸酯化合物。A simple and general method for the synthesis of polyfluoroethylene malonates was developed,which was achieved by Knoevenagel reaction of polyfluoroacetaldehydes hemiacetals with malonates.It was found polyfluoroacetaldehyde hemiacetal substrates could be readily available more easily by the reduction of ethyl polyfluoroacetate.Then the effect of base,acid catalysts,solvents and catalyst dosage on the reaction yield were examined respectively.The results showed that the optimized conditions used 30 mol%of piperidine and acetic acid as the catalysts,toluene as the solvent,and heated to reflux for 24 hours.Under these conditions,a series of polyfluoroacetaldehyde hemiacetals and malonates were employed for the Knoevenagel reactions and obtained the corresponding polyfluoroethylene malonates in the moderate yield.

关 键 词：KNOEVENAGEL反应 多氟亚乙基丙二酸酯 三氟甲基 半缩醛 哌啶 

分 类 号：O62[理学—有机化学]