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机构地区:[1]襄樊学院化学工程与食品科学学院,湖北襄樊441053 [2]武汉工程大学湖北省新型反应器与绿色化学工艺重点实验室,湖北武汉430074
出 处:《化学世界》2011年第6期355-358,共4页Chemical World
摘 要:以辛溴烷、苯酚和碘苯等为原料,在十六烷基三甲基溴化铵的催化作用下制备了苯基正辛基醚,苯基正辛基醚与碘苯经过氧乙酸氧化,对甲苯磺酸成盐得到(4-辛烷氧基苯基)苯碘鎓对甲苯磺酸盐。最佳反应条件为:碘苯、辛烷氧基苯和过氧乙酸的摩尔比为1∶1∶2.2;反应温度40℃;反应时间为12 h。在丙酮溶剂中,(4-辛烷氧基苯基)苯碘鎓对甲苯磺酸盐与六氟锑酸钾进行离子交换得到目的产物(4-辛烷氧基苯基)苯碘鎓六氟锑酸盐。通过紫外光谱、红外光谱和核磁共振测定,对产物进行了结构确证。总收率为62.7%。A method was provided for preparing(4-octyloxyphenyl)phenyl iodonium hexafluoroantimonate salt.n-Octylphene ether was initially synthesized using 1-bromooctane and phenol in the presence of hexadecyltrimethylammonium bromide which was acted as phase transfer catalyst followed by the addition of iodobenzene,peracetic acid,and p-toluene sulfonic acid.The optimum reaction conditions were as follows:iodobenzene,n-octylphene ether and peracetic acid ratio was 1∶1∶2.2,reaction time was 12 h and reaction temperature was 40℃.The resulting(4-octyloxyphenyl)phenyl iodonium tosylate reacted with KSbF6 in the solution of acetone to give the(4-octyloxyphenyl)phenyliodonium hexafluoroantimonate,whaoe structure was identified by UV,IR and H NMR.The total yield was above 62.7%.
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