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机构地区:[1]临沂大学生命科学学院,山东临沂276000 [2]东华大学化学化工与生物工程学院,上海201620 [3]嘉兴学院材料与纺织工程学院,浙江嘉兴314001
出 处:《精细化工》2013年第10期1173-1176,共4页Fine Chemicals
摘 要:以氢氧化钠水溶液为水相,采用液-液相转移催化方法,通过Wittig-Horner反应合成二苯乙烯。考察了催化剂种类、催化剂用量、水相碱液质量分数、反应温度、有机相溶剂种类对转化率的影响,并比较不同种类的醛在液液相转移催化体系中的反应性。结果表明,以四辛基溴化铵为相转移催化剂、n(相转移催化剂)∶n(磷酸酯)=1∶10、水相碱液质量分数为50%、反应温度45℃、甲苯为有机相溶剂,二苯乙烯的收率可达94%;不同种类的醛为原料时,相转催化Wittig-Horner反应均有较高的收率并且产物结构以E式为主。Stilbene was synthesized via Wittig-Homer reaction in liquid-liquid phase-transfer catalysis (LL-PTC) system in which NaOH aqueous solution and nonpolar solvent were used as the aqueous phase and the organic solvent, respectively. The effect of the various catalysts, the amount of catalyst, the mass fraction of NaOH, the temperature and the various solvents on the conversion rate were investigated. The activity of various aldehydes for Wittig-Horner reaction in LL-PTC system was also investigated. The optimum reaction conditions were ascertained as follows :tetraoctyl ammonium bromide ( TOAB ) as phase transfer catalyst, n ( TOAB ) :n (phosphonate) = 1 : 10, mass fraction of NaOH aqueous solution 50% , at 45 ℃ and toluene as solvent. The isolated yield was more than 94% under these optimum reaction conditions. Wittig-Horner reaction gave a high isolated yield and geometric selectivity (E-isomer) for various aldehydes in LL-PTC system.
关 键 词:二苯乙烯 液液相转移催化 WITTIG-HORNER反应 精细化工中间体
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