【摘要】 以烯丙基氯与金属镁反应制得烯丙基氯化镁,再与原甲酸三乙酯反应,合成了3-丁烯醛缩二乙醇。研究了反应条件对反应的影响,确定了反应的最佳工艺条件:在乙醚中,-10～-5℃,n(镁粉)∶n(烯丙基氯)=1.0∶1.0反应,制得了烯丙基氯化镁,收率80%;将烯丙基氯化镁与原甲酸三乙酯按物质的量比1∶1反应,回流6h,用饱和氯化铵水溶液水解,蒸除乙醚,再减压蒸馏,制备了3-丁烯醛缩二乙醇,收率75.6%,含量98%以上。产品经元素分析、核磁共振、红外光谱等进行了确认。更多还原

【Abstract】 3-Butenal diethyl acetal was prepared by the reaction of triethyl orthoformate with allylmagnesium chloride obtained by the reaction based on magnesium and allyl chloride.Factors influencing on the reaction were studied and the following optimum conditions were determined,i.e.using ether as solvent,allylmagnesium chloride was prepared with mass ratio of n(magnesium poder)∶n(allyl chloride)=1.0∶1.0 at-10～-5℃,the yield was 80%.Then the following procedures were carried out to prepare 3-butenal diethyl acetal,i.e.reacting allylmagnesium with triethyl orthoformate in 1∶1 of mass ratio,refluxing for 6 hours,hydrolysis with saturated aqueous ammonium chloride,then distilling under reduced pressure after the ether was distilled off,the yield of title compound was 75.6% with content over 98%.The final product was confirmed by elementary analysis,IR and 1HNMR.更多还原