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作 者:肖亮[1] 曹靖[1] 阳年发[1] 杨利文[1] 刘百炼[1]
出 处:《精细化工》2005年第11期869-870,共2页Fine Chemicals
基 金:国家自然科学基金资助项目(20472069)~~
摘 要:以烯丙基溴为原料,在N2保护下,乙醚中与镁反应30 m in制得烯丙基溴化镁的乙醚溶液(Ⅰ)。过滤后,将Ⅰ从45℃逐步加热到65℃,蒸出乙醚。然后快速加入四氢呋喃(THF),65℃搅拌20 m in,制得烯丙基溴化镁的THF溶液(Ⅱ)。在冰浴中向Ⅱ缓慢滴加氯代三苯甲烷的THF溶液,搅拌3 h,制得4,4,4-三苯基-1-丁烯(Ⅲ),收率93%。用红外光谱、核磁共振氢谱和碳谱对产物进行了表征。Diethyl ether solution of allylmagnesium bromide(Ⅰ) was prepared by stirring allyl bromide with magnesium in dry diethyl ether under N2 for 30 min. After filtration, diethyl ether was removed from Ⅰby raising the temperature from 45℃ to 65℃ progressively. Dry tetrahydrofuran (THF) was then added rapidly to the gray pasty residue, and the mixture was stirred at 65℃ for 20 min to give THF solution of allyl magnesium bromide(Ⅱ). Then the THF solution Ⅱ was cooled in an ice bath, and a THF solution of triphenylmethyl chloride was slowly dropped into it with stirring for 3 h. 4,4,4- Triphenyl-1-butene(Ⅲ) was synthesized in 93% yield. Structure of the product Ⅲ was identified by IR,^1HNMR and ^13 CNMR.
关 键 词:烯丙基 三苯甲基 4 4 4-三苯基-1-丁烯
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